반응식
C([N:14]1[CH2:17][CH:16]([N:18]2[CH2:23][CH2:22][N:21]([C:24](=[O:29])[C:25]([F:28])([F:27])[F:26])[CH2:20][CH2:19]2)[CH2:15]1)(C1C=CC=CC=1)C1C=CC=CC=1.ClC(OC(Cl)C)=O.CO.CCOCC>C(Cl)Cl>[NH:14]1[CH2:15][CH:16]([N:18]2[CH2:19][CH2:20][N:21]([C:24](=[O:29])[C:25]([F:26])([F:27])[F:28])[CH2:22][CH2:23]2)[CH2:17]1참가 물질
6
반응 조건
- 온도
- 0 °C
실험 절차
To a solution of compound 1f (2.11 g, 5.23 mmol) in CH2Cl2 (60 mL) was added 1-chloroethyl chloroformate (2.0 mL, 18.35 mmol) at 0° C. under N2. The mixture was stirred at 0° C. for 90 min and then MeOH (4 mL) was added. The mixture was refluxed for 1 h. Upon cooling, Et2O (50 mL) was added to the mixture. The resulting solid was collected by filtration and dried. The crude compound 1g was used in the next reaction without further purification. MS m/z (M+H+) 238.1.
후처리
- temperatureThe mixture was refluxed for 1 h
- temperatureUpon cooling
- filtrationThe resulting solid was collected by filtration
- customdried
- customThe crude compound 1g was used in the next reaction without further purification
출처 및 근거
- ORD 기록
- ord-e527049969ac4bbb9818c629d2bcc86d
- 출처 데이터셋
- uspto-grants-2013_12
- 특허 번호
- US08604017B2
연결된 노트
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