CARBON TETRACHLORIDE.10 Vol

Dimethylthiocarbamyl chloride can be prepared as described in Org. Syn., Coll. Vol. 4, 310 (1963), or by rapidly adding 740 g. (10.5 moles) of chlorine dissolved in 3 1. of carbon tetrachloride to a stirred refluxing suspension of 2400 g. (10 moles) of tetramethylthiram disulfide (Note 9) in 5 1. of carbon tetrachloride. After the addition is complete, approximately one-half of... 

The AcOVE polymerization reaches approximately 100% conversion after 50 min, at which moment 1.0 mL of an IBVE solution is added with the mixture kept at - 15° C. The IBVE solution has been prepared beforehand by mixing IBVE (0.66 mL), carbon tetrachloride (0.64 mL the internal standard for GC), and toluene (8.7 mL) thus, the AcOVE/ IBVE mole ratio = 30 10 in the reaction mixture. After an additional 35 min, where IBVE conversion reaches about 100%, the second stage polymerization is terminated at - 15° C with 2.0 mL of prechilled methanol containing about 2 vol% aqueous ammonia. 

Sixteen grams (0.10 mole) of bromine is added gradually with stirring to a solution of 20 g. (0.10 mole) of phenoxathiin [Org. Syntheses Coll. Vol. 2, 485 (1943)] in 100 ml. of carbon tetrachloride. (Hood.)... 

To a solution of 42 g. (0.23 mole) of benzhydrol [Org. Syntheses Coll. Vol. 1, 90 (1941)] in 125 g. of carbon tetrachloride is added slowly 27 g. (0.10 mole) of phosphorus tribromide. The mixture is allowed to stand for a day and then is heated to 60-70° for 6 hours. The reaction mixture is filtered, washed with ice water then with dilute sodium acetate solution, dried over calcium chloride, and distilled. The diphenylmethyl bromide is obtained in 65% yield (36 g.) boiling at 172-176°/14 mm. and melting at 43-45°. 

Figure 4. Dose-response curve for carbon tetrachloride-induced liver injury in male rats. The carbon tetrachloride was dissolved in corn oil and doses of 0 (controls), l, 10, and 33 mg/kg b.w. were administered 5 dayslweek for 12 weeks. Severe liver injury was observed in all animals at the highest dose, but only relatively mild changes (increased liver weights) were seen at 10 mg/kg b.w. No differences of any type were observed between the control and low dose animals. The dose of 1 mg/kg b.w. is thus a NOEL for this species and this period of dosing. Data were reported by J.V. Bruckner and co-workers in 1986 in Fundamental and Applied Toxicology, Vol. 6 (No. 1), pages 16—34.

The preparation of dichloro enitol 7 by treatment of tetra-O-benzyl-D-glucono-6-lactone with tris (dimethylamino) phosphine-carbon tetrachloride has been reported. (See Vol. 25, p. 155 Scheme 10 for similar work.)... 

The transformation of aldonolactones into the corresponding dichloromethylene derivatives on reaction with triphenylphosphine-carbon tetrachloride reagent has been described (Scheme 10). This reagent is of more general applicability than the bis(dimethylamino)phosphine-carbon tetrachloride reported earlier (Vol. 18, p.34). Ester carbonyl groups are also dichloromethylated. 

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