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Water → 1-[2,4-Bis(trifluoromethyl)benzyl]-5-(hydroxymethyl)azepan-2-one

HRID 1620634
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인쇄 미리보기

반응식

HRID 1620634 반응식
[F:1][C:2]([F:28])([F:27])[C:3]1[CH:22]=[C:21]([C:23]([F:26])([F:25])[F:24])[CH:20]=[CH:19][C:4]=1[CH2:5][N:6]1[C:12](=[O:13])[CH2:11][CH2:10][CH:9]([C:14](OCC)=[O:15])[CH2:8][CH2:7]1.[BH4-].[Li+].O>C1COCC1>[F:28][C:2]([F:1])([F:27])[C:3]1[CH:22]=[C:21]([C:23]([F:26])([F:25])[F:24])[CH:20]=[CH:19][C:4]=1[CH2:5][N:6]1[CH2:7][CH2:8][CH:9]([CH2:14][OH:15])[CH2:10][CH2:11][C:12]1=[O:13]
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참가 물질

5

반응물 3

HCID 962WaterHCID 4148881Lithium borohydrideHCID 86678800Ethyl 1-[2,4-bis(trifluoromethyl)benzyl]-7-oxoazepane-4-carboxylate

생성물 1

HCID 866788011-[2,4-Bis(trifluoromethyl)benzyl]-5-(hydroxymethyl)azepan-2-one수율 90.3%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
50 °C

실험 절차

To a solution of ethyl 1-[2,4-bis(trifluoromethyl)benzyl]-7-oxoazepane-4-carboxylate (14.8 g) in THF (400 mL) was added lithium borohydride (4.5 g). The reaction mixture was stirred at 50° C. for 1 hr, water was added, and the mixture was extracted with ethyl acetate. The extract was dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure to give the title compound (12.0 g).

후처리

  1. extractionthe mixture was extracted with ethyl acetate
  2. dry with materialThe extract was dried over anhydrous sodium sulfate
  3. customthe solvent was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-395a40ceaad646bfaf3a6e47f2fc35d9
출처 데이터셋
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08772277B2

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