Trichloroacetyl chloride → HCID 59432914, 화합물
반응식
[Cl:1][C:2]([Cl:7])([Cl:6])[C:3](Cl)=[O:4].[CH2:8]1[C:16]2[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=2)[CH2:10][NH:9]1.CCN(CC)CC>C(Cl)Cl>[Cl:1][C:2]([Cl:7])([Cl:6])[C:3]([N:9]1[CH2:10][C:11]2[C:16](=[CH:15][CH:14]=[CH:13][CH:12]=2)[CH2:8]1)=[O:4]참가 물질
5
실험 절차
Under N2, at 0° C., trichloroacetyl chloride (0.57 mL, 5.0 mmol) was added dropwise to a stirring solution of isoindoline (1.0 g, 5.0 mmol), Et3N (0.7 mL, 0.51 g, 5.0 mmol) and CH2Cl2 (20 mL). The solution was allowed to warm to room temperature and stirred for 1 h. After evaporating the solvents in vacuo, the mixture was purified via silica gel chromatography using 8:2 hexanes/EtOAc to obtain the desired amide (1.2 g, 4.6 mmol, 91% yield). LC/MS (10-99% CH3CN), M/Z: M+1 obs=265.9; tR=3.51 min.
후처리
- customAfter evaporating the solvents in vacuo
- customthe mixture was purified via silica gel chromatography
출처 및 근거
- ORD 기록
- ord-ac0712c477d04e709ea57f6f98ce543d
- 출처 데이터셋
- uspto-grants-2010_08
- 특허 번호
- US07786137B2
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