Butyl sulphite

Fit up the apparatus shown in Fig. Ill, 31,1 the capacity of the Claisen flask should be 100 ml. Place 40 g. (24 5 ml.) of redistilled thionyl chloride in the flask and 50 g. (62 ml.) of dry n-butyl alcohol (b.p. 116-117°) in the dropping funnel. Cool the flask in ice and add the n-butyl alcohol, with quent shaking, over 1 hour (1). Reflux the mixture gently for 1 hour to complete the reaction and to remove the residual hydrogen chloride. Arrange the apparatus for distillation, and distil under normal pressure until the temperature rises to 120° then distil under diminished pressure (Fig. II, 20,1) and collect the di-n-butyl sulphite at 116—118°/20 mm. The yield is 55 g. 

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Di-n-butyl ether. Technical n-butyl ether does not usually contain appreciable quantities of peroxides, unless it has been stored for a prolonged period. It should, however, be tested for peroxides, and, if the test is positive, the ether should be shaken with an acidified solution of a ferrous salt or with a solution of sodium sulphite (see under Diethyl ether). The ether is dried with anhydrous calcium chloride, and distilled through a fractionating column the portion, b.p. 140-141°, is collected. If a fraction of low boiling point is obtained, the presence of n-butyl... 

Annex III lays down the conditions of use for permitted preservatives and antioxidants, with lists of foods and maximum levels in each case. Part A lists the sorbates, benzoates and p-hydroxybenzoates, E 200-E 219 part B lists sulphur dioxide and the sulphites, E 220-E 228 part C lists other preservatives with their uses, including nisin, dimethyl dicarbonate and substances allowed for surface treatment of certain fruits, E 249 potassium nitrite, E 250 sodium nitrite, E 251 sodium nitrate and E 252 potassium nitrate, E 280-E 283 propionic acid and the propionates part D lists the antioxidants E 320 butylated hydroxyanisole (BHA), E 321 butylated hydroxytoluene (BHT), E 310 propyl gallate, E 311 octyl gallate, E 312 dodecyl gallate, E 315 eiythorbic acid and E 316 sodium erythorbate. 

CHLOROETHYL-P -(p-tert-BUTYLPHENOXY)-a -METHYLETHYL SULFITE P-CHLOROETHYL-P-(p-tert-BUTYLPHENOXY)-a-METHYLETHYL SULPHITE 2-CHLOROETHYL l-METHYL-2-(p-tert-BUTYL-PHENOXY)ETHYL SULPHITE 2-CHLOROETHYL SULFUROUS ACID-2-(4-(l,1-DIMETHYLETHYL-)PHENOXY)-l-METHYLETHYL ESTER 2-CHLORO-ETHYL SULPHITE of l-(p-tert-BUTYLPHENOXY)-2-PROPANOL COMPOUND 88R ENT 16,519 NIAGARAMITE ORTHO-MITE 88-R... 

Sulphur. Irradiation of tetrachloro-l,2-benzoquinone is reported to give the sulphate 18 (53LA199). The sulphite 19 is formed in 72% )deld by treatment of the di-fert-butyl derivative with Ir(PiPr3)2(SO)Q (87ZNB799). 

Cyclic sulphinamates (205), like cyclic sulphites, also prefer a chair conformation with an axial S=0 group. Substituents R on the nitrogen atom are preferentially axial. The 3-t-butyl-cw-4-methyl derivative (206) has been shown to prefer (in solution and in the solid state) a slightly distorted chair conformation, with nitrogen at the top of a very flattened pyramid, with axial S=0 and methyl, and with the t-butyl group displaced towards the axial direction. Unlike cyclic sulphites, the chair form with equatorial S=0 is rarely involved, and twist forms with a 3,6- or 1,4-axis were observed. Carbon-13 n.m.r. spectra of the five-membered analogues (207) have also been related to the conformational situation. ... 

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