Allyl Mercaptan → HCID 20143887, compound

Into a 1 liter flask equipped with cooling bath, thermometer, reflux condenser and additional funnel as well as electric stirrer is placed 68.2 grams of methyl-4-chlorobutyrate. The methyl-4-chlorobutyrate is cooled to 20° C. The mixture of sodium methoxide and allyl mercaptan is added to the addition funnel. Over a period of 0.5 hours while maintaining the pot temperature at 20°-30° C., the mixture of allyl mercaptan and sodium methoxide is added slowly to the methyl-4-chlorobutyrate with stirring. The reaction is exothermic and requires slight cooling. At the end of the addition of the mixture of allyl mercaptan and sodium methoxide, the reaction mass is stirred for 1 hour and the temperature of the reaction mass is permitted to rise to 38° C. 500 ml water are then added to the reaction mass and the reaction mass is transferred to a separatory funnel. The reaction mass is then extracted with three 50 ml portions of methylene dichloride and dried over anhydrous sodium sulfate and filtered. The reaction mass is then distilled on a micro Vigreux column yielding the following fractions:

1. customInto a 1 liter flask equipped
2. temperaturewith cooling bath
3. temperaturethermometer, reflux condenser and additional funnel as well as electric stirrer
4. additionis added to the addition funnel
5. temperatureOver a period of 0.5 hours while maintaining the pot temperature at 20°-30° C.
6. stirringthe reaction mass is stirred for 1 hour
7. customto rise to 38° C
8. customthe reaction mass is transferred to a separatory funnel
9. extractionThe reaction mass is then extracted with three 50 ml portions of methylene dichloride
10. dry with materialdried over anhydrous sodium sulfate
11. filtrationfiltered
12. distillationThe reaction mass is then distilled on a micro Vigreux column
13. customyielding the following fractions

ORD record

ord-9a77734ffd654bfdaba0e8020b545b27

Source dataset

uspto-grants-1988_04

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04739105