Trifluoroacetic acid → (3R,6S)-3-Amino-6-(2,3-difluorophenyl)-1-pyridin-4-ylazepan-2-one

HRID 501146

반응식

HRID 501146 반응식
FC(F)(F)C(O)=O.[F:8][C:9]1[C:14]([F:15])=[CH:13][CH:12]=[CH:11][C:10]=1[C@H:16]1[CH2:22][N:21]([C:23]2[CH:28]=[CH:27][N:26]=[CH:25][CH:24]=2)[C:20](=[O:29])[C@H:19]([NH:30]C(=O)OC(C)(C)C)[CH2:18][CH2:17]1>ClCCl>[NH2:30][C@@H:19]1[CH2:18][CH2:17][C@@H:16]([C:10]2[CH:11]=[CH:12][CH:13]=[C:14]([F:15])[C:9]=2[F:8])[CH2:22][N:21]([C:23]2[CH:24]=[CH:25][N:26]=[CH:27][CH:28]=2)[C:20]1=[O:29]

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 86595044tert-Butyl (3R,6S)-6-(2,3-difluorophenyl)-2-oxo-1-pyridin-4-ylazepan-3-ylcarbamate

생성물 1

HCID 60037853(3R,6S)-3-Amino-6-(2,3-difluorophenyl)-1-pyridin-4-ylazepan-2-one

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Trifluoroacetic acid (2 mL) was added to a solution of tert-butyl (3R,6S)-6-(2,3-difluorophenyl)-2-oxo-1-pyridin-4-ylazepan-3-ylcarbamate (55 mg, 0.132 mmol) in dichloromethane (2 mL). After 1 h, the solution was concentrated. Saturated aqueous sodium bicarbonate solution was added and the mixture was extracted with dichloromethane (3×). The combined organic extracts were washed with saturated brine, dried over magnesium sulfate, filtered and concentrated. MS 318.2 (M+1).

후처리

  1. concentrationthe solution was concentrated
  2. additionSaturated aqueous sodium bicarbonate solution was added
  3. extractionthe mixture was extracted with dichloromethane (3×)
  4. washThe combined organic extracts were washed with saturated brine
  5. dry with materialdried over magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-aa5ff3cecf674ee8a13ce8792a1c3e8c
출처 데이터셋
uspto-grants-2010_08
특허 번호
US07772224B2

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