3-MERCAPTO-3-METHYL-1-BUTYL-1-FORMATE synthesis

Yield: 21.5 g (90%)

Reaction Conditions:

with pyridine;formic acid;acetic anhydride

Steps:

III Preparation of 3-mercapto-3-methylbutyl formate
EXAMPLE III Preparation of 3-mercapto-3-methylbutyl formate A mixture of 21.5 g of acetic anhydride and 10.8 g of formic acid was heated at 45°C for 11/2 hours. After cooling 1.7 g of pyridine was added and, with stirring, 19.5 g of 3-mercapto-3-methylbutyl alcohol in the course of 5 minutes. The temperature of the reaction mixture slowly rose to 45°C. After completion of the addition, the reaction mixture was held at 45°C for 4 hours and then cooled to room temperature. It was dissolved in ether, washed five times with 3% aqueous NaHCO₃ solution and finally with NaCl solution to neutral. The ethereal solution was dried over sodium sulphate, filtered and concentrated. Distillation of the residue yielded 21.5 g (90%) of 3-mercapto-3-methylbutyl formate b.p. 30°-31°C/1 mm, n_D²⁰ 1.4610.

References:

Polak's Frutal Works B.V.;Douwe Egberts Koninklijke Tabaksfabriek-Koffiebranderijen-Theehandel N.V. US3970689, 1976, A