Hexane → Thiophene, 3-methoxy-2-(methylthio)-
반응식
[CH3:1][O:2][C:3]1[CH:7]=[CH:6][S:5][CH:4]=1.CCCCCC.C([Li])CCC.[CH3:19][S:20]SC>C(OCC)C.O>[CH3:19][S:20][C:4]1[S:5][CH:6]=[CH:7][C:3]=1[O:2][CH3:1]참가 물질
7
반응 조건
- 온도
- -78 °C
실험 절차
To a stirred solution of 21 g of 3-methoxythiophene in diethyl ether at -40° C. was added 115 ml of a 1.6 molar hexane solution of n-butyllithium. The mixture was warmed slowly over 10 minutes to 0° C., then refluxed for 1 hour, was cooled to -78° C. and a solution containing 21.4 g of dimethyldisulphide in 100 ml of diethyl ether was added. The reaction mixture was warmed to room temperature and stirred for 30 minutes, was poured into water and the organic layer washed with water, with brine, and was then dried over magnesium sulphate and evaporated to dryness.
후처리
- temperatureThe mixture was warmed slowly over 10 minutes to 0° C.
- temperaturerefluxed for 1 hour
- additionwas added
- temperatureThe reaction mixture was warmed to room temperature
- washthe organic layer washed with water, with brine
- dry with materialwas then dried over magnesium sulphate
- customevaporated to dryness
출처 및 근거
- ORD 기록
- ord-9e381083e85f47378f157bd737f1197c
- 출처 데이터셋
- uspto-grants-1988_04
- 특허 번호
- US04738959
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