تفاعل #71583

معادلة التفاعل

ethyl tiglate

thioacetic acid

para-toluenesulfonic acid

sodium bicarbonate

→

objective compound

المردود 93.4%

ethyl 3-acetylthio-2-methylbutyrate

المردود 93.4%

المذيبات

diethyl ether

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةAfter cooling
2. 2
   أخرىThe organic layer was separated
3. 3
   غسيلwashed twice with brine
4. 4
   أخرىThe solvent in the organic layer was evaporated off
5. 5
   workup.DISTILLATIONvacuum distillation (68 to 71° C./2 torr)

الإجراء التجريبي

A mixture of 51.27 g (0.40 mol) of ethyl tiglate, 76.12 g (1.00 mol) of thioacetic acid, and 7.60 g (0.04 mol) of para-toluenesulfonic acid was stirred under nitrogen atmosphere at 75° C. for 24 hours. After cooling, diethyl ether and a saturated aqueous sodium bicarbonate solution were added to the reaction mixture. The organic layer was separated and washed twice with brine. The solvent in the organic layer was evaporated off, and vacuum distillation (68 to 71° C./2 torr) was performed to give 76.36 g of the objective compound (GC purity: 98.3%, yield: 91.8%, diastereomer ratio: 80.9/19.1).

المصدر