Ethanol → HCID 178517499, 화합물
반응식
Br[CH2:2][C:3]([C:5]1[CH:10]=[CH:9][C:8]([F:11])=[CH:7][CH:6]=1)=O.[S-:12][C:13]#[N:14].[Na+].C([OH:18])C>>[F:11][C:8]1[CH:9]=[CH:10][C:5]([C:3]2[N:14]=[C:13]([OH:18])[S:12][CH:2]=2)=[CH:6][CH:7]=1참가 물질
4
반응 조건
- 온도
- 100 °C
실험 절차
1.085 g (5 mmol) of 2-bromo-1-(4-fluoro-phenyl)-ethanone and 405 mg (5 mmol) of sodium thiocyanate in 40 ml of ethanol were heated under reflux for 30 min. Then 20 ml of ethanol were distilled off, water was added, the precipitate was filtered off, 10 ml of acetic acid, 0.5 ml of water and 0.2 ml of concentrated sulfuric acid were added, and the mixture was stirred at 100° C. for 1 h. After dilution with water, the precipitated product was filtered off, washed with water and dried. Yield: 782 mg.
후처리
- temperatureunder reflux for 30 min
- distillationThen 20 ml of ethanol were distilled off
- additionwater was added
- filtrationthe precipitate was filtered off
- addition10 ml of acetic acid, 0.5 ml of water and 0.2 ml of concentrated sulfuric acid were added
- filtrationAfter dilution with water, the precipitated product was filtered off
- washwashed with water
- customdried
출처 및 근거
- ORD 기록
- ord-2bbfaaeeca27455a9cbc468af86954ed
- 출처 데이터셋
- uspto-grants-2012_05
- 특허 번호
- US08188291B2
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