Sodium hydride → HCID 86759694, 화합물

HRID 2179957

반응식

HRID 2179957 반응식
[H-].[Na+].[OH:3][CH:4]([C:15]1[CH:16]=[N:17][CH:18]=[CH:19][CH:20]=1)[CH2:5][CH2:6][NH:7][C:8](=[O:14])[O:9][C:10]([CH3:13])([CH3:12])[CH3:11].[Cl:21][C:22]1[C:29]([F:30])=[CH:28][C:25]([C:26]#[N:27])=[C:24](F)[CH:23]=1>O1CCCC1>[Cl:21][C:22]1[C:29]([F:30])=[CH:28][C:25]([C:26]#[N:27])=[C:24]([CH:23]=1)[O:3][CH:4]([C:15]1[CH:16]=[N:17][CH:18]=[CH:19][CH:20]=1)[CH2:5][CH2:6][NH:7][C:8](=[O:14])[O:9][C:10]([CH3:13])([CH3:12])[CH3:11]

참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 112753024-CHLORO-2,5-DIFLUOROBENZONITRILEHCID 69799429[3-Hydroxy-3-(3-pyridinyl)propyl]carbamic acid 1,1-dimethylethyl ester

생성물 1

HCID 86759694HCID 86759694, 화합물수율 88%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Sodium hydride (141 mg, 60% dispersion in oil) was added to a solution of the product from step (b) (785 mg, 2.96 mmol) and 4-chloro-2,5-difluorobenzonitrile (546 mg, 3.75 mmol) in tetrahydrofuran (9 ml) and the resultant suspension was stirred for 0.5 h. The mixture was quenched with saturated aqueous ammonium chloride, basified to pH 8 and extracted with ethyl acetate (three times). The combined organic extracts were dried (sodium sulphate), evaporated and purified by chromatography on silica eluting with petrol—acetone to give 1.05 g (88%) of the sub-title compound as a colourless oil.

후처리

  1. customThe mixture was quenched with saturated aqueous ammonium chloride
  2. extractionextracted with ethyl acetate (three times)
  3. dry with materialThe combined organic extracts were dried (sodium sulphate)
  4. customevaporated
  5. custompurified by chromatography on silica eluting with petrol—acetone

출처 및 근거

ORD 기록
ord-e90cccf4c60846e3b9d4703c2fbf62f6
출처 데이터셋
uspto-grants-2005_05
특허 번호
US06887871B2

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