Tartaric acid, evaporating

The united filtrate is evaporated on the steam bath until the volume amounts to 200 cc., at which point crystals should have already begun to separate from the hot solution. After standing at room temperature for twenty-four hours or longer, the crystals are filtered by suction as free from mother liquor as possible and recrystallized from an equal weight of distilled water (Note 5). The filtrate from this recrystallization is evaporated on the steam bath and the second crop of /-tartaric acid filtered and recrystallized as before. The -yield is 65-75 (32-5-35-5 per cent of the theoretical amount). 

Stirring is carried out first for 3 hours at room temperature and then for 2 hours at boiling temperature, it is then cooled and poured into 300 ml of ice-cold 20% ammonium chloride solution. It is then shaken out with methylene chloride, the methylene chloride solution washed with water and shaken 3 times with 30 ml portions of aqueous 2N tartaric acid solution. The tartaric acid extract is rendered alkaline while cooling thoroughly and then extracted twice with methylene chloride. After washing with water, drying over potassium carbonate and reducing in volume by evaporation, the residue is recrystallized from ethanol. MP 197° to 199°C. 

The undistilled aqueous tartaric acid solution was extracted with three 1-liter portions of ethyiene dichloride, and was then brought to a pH of about 8.5 to 9.5 by the addition of 28% aqueous ammonium hydroxide. The ammoniacal solution was extracted with three 1-liter portions of ethylene dichloride the ethylene dichloride extracts were combined, were dried, and were evaporated in vacuo, yielding a residue of 3.35 grams of a iight-brown powder. 

Finely grind seeds (preferably woodrose) and add NaHC03. Extract with ethyl acetate by soaking about one day. Filter and extract the ethyl acetate with tartaric acid solution. Basify the extract with NaHCOj and extract it with ethyl acetate. Dry and evaporate in vacuum the ethyl acetate to get the alkaloids. Repeat this procedure on the seeds until no more residue is obtained. 

Evaporate the chloroform extracts and dissolve the residue in the minimum amount of a 3% tartaric acid solution. If all the residue doesn t dissolve, place it into suspension by shaking vigorously. 

Extract again with alcoholic tartaric acid and evaporate in a vacuum to dryness. The dry material is the salt (i.e., the tartaric acid salt, the tartrate) of the ergot alkaloids, and is stored in this form because the free basic material is too unstable and decomposes readily in the presence of light, heat, moisture and air. 

Add 1.16 g ergotamine.HCl to 4 ml anhydrous hydrazine and heat one hour at 90°. Add 20 ml water and evaporate in vacuum. Can proceed to the next step or can purify by adding ether and aqueous tartaric acid, basify the aqueous phase and extract aqueous phase with CHC13 to get mainly d-iso-lysergic hydrazide (I). Can... 

The aqueous hydrazide solution is evaporated from a tared 2000 ml flask on an efficient rotary evaporator, using a bath temperature of 40° and an ice-cooled condenser the 3000 ml siphon flask assembly is used as storage for the vacuum feed. The weight of the crude hydrazide so obtained is determined, it is dissolved in about 170 ml 1 N tartaric acid, the aqueous solution washed with three 30 ml portions ether, made alkaline with 190 ml 1 N ammonium hydroxide, and exhaustively extracted with successive portions of chloroform, the first two portions being 100 ml each, the following 50 ml. 

In 1770 C. W. Scheele showed that the natural product cream of tartar is a salt with a vegetable alkaline base (potash) supersaturated with a vegetable acid (tartaric). When he dissolved cream of tartar [potassium acid tartrate] in boiling water and added powdered chalk to the solution, the lime combined with part of the tartaric acid and gave a copious white precipitate. On evaporating the supernatant liquid he obtained crystals of soluble tartar [normal potassium tartrate] (9, 10). 

S-(—)-l-(2-Pyridyl)ethylamine.22 To a 1-L Erlenmeyer flask 34.5 g (0.230 mole) of L-(+)-tartaric acid in 220 mL of boiling 95% EtOH is added 23.6 g (0.193 mole) of racemic l-(2-pyridyl)ethylamine in 300 mL of hot 95% EtOH. As the solution cools to ambient temperature and is allowed to sit for several hours, a white precipitate forms. Four recrystallizations of this precipitate from 100 mL of 95% EtOH gives 12.9 g of the (+)-acid tartrate salt of S-( —) amine (> 99% ee). The salt is neutralized by dissolving in 250 mL of 2 NNaOH and extracting with four 150-mL portions of ether. The organic layer is dried over solid NaOH and then concentrated by rotary evaporation. 

Tartrate Ammonium tartrate [CAS 3164-29-2] (NH4)2C4kLOb. white solid, moderately soluble, formed by reaction of NH4OH and tartaric acid, and then evaporating. Used in the textile industry ammonium hydrogen tartrate, ammonium bitartrate, ammonium acid tartrate NH4HC4H4CX , white solid, slightly soluble, formation sometimes used in detection of ammonium or tartrate. 

Ether defatting. Multiple extraction with 1,2-dichloroethane, aqueous solution pH = 10, tartaric acid, H2S04, NaOH, CHCI3. Evaporation at 40°C. 

Powders with a tartaric acid basis are tested for as follows About 20 grams of the powdered bread are treated with water in a flask of about 200 c.c. capacity on a water-bath, the liquid being concentrated to about 50 c.c., transferred to a separating funnd, acidified with sulphuric add and extracted with ether. The ethereal solution is evaporated in a porcelain dish and the residue heated with a few crystals of resorcinol and one or two drops of concentrated sulphuric acid until white fumes appear the formation of a violet-red coloration indicates the presence of tartaric add. 

To ascertain if the precipitate is really cream of tartar, the following test, due to D6nig6s, is used When the crystalline precipitate has settled, the supernatant liquid is decanted off and the precipitate washed with a fine stream of alcohol into a dish, the excess of alcohol being then evaporated. Some of the remaining crystals arc introduced into a test-tube containing 3 c.c. of concentrated sulphuric acid and 3 drops of a resorcinol solution prepared by dissolving 2 grams of pure resorcinol in 100 cc. of water acidified with 5 CjC. of sulphuric acid. The solution is heated to 130-140° in presence of tartaric acid, a distinct carmine coloration is produced. 

The 3-chloro-l-(4-indolyloxy)-2-propanol is dissolved in 50 ml of toluene and 50 ml of isopropylamine and heated to the boil for 45 h. Evaporation to dryness is effected in a vacuum, the residue is shaken out thrice between ethyl acetate and a 1 N tartaric acid solution and a 5 N sodium hydroxide solution is then added to the combined tartaric acid phases until an alkaline reaction is obtained. The alkaline solution is shaken out thrice with 50 ml of methylene chloride, the extracts are dried over magnesium sulfate and the solvent evaporated in vacuum. The residue is crystallized from ethyl acetate/ether to give the 4-(2-hydroxy-3-isopropylaminopropoxy)indole. 

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