Acetyl chloride → HCID 44359309, 화합물
반응식
Cl.[NH2:2][CH2:3][CH:4]([C:6]1[C:15]2[C:10](=[CH:11][CH:12]=[C:13]([O:16][CH3:17])[CH:14]=2)[CH:9]=[CH:8][CH:7]=1)[OH:5].C(=O)([O-])[O-].[K+].[K+].[C:24](Cl)(=[O:26])[CH3:25]>O.C(OCC)(=O)C>[OH:5][CH:4]([C:6]1[C:15]2[C:10](=[CH:11][CH:12]=[C:13]([O:16][CH3:17])[CH:14]=2)[CH:9]=[CH:8][CH:7]=1)[CH2:3][NH:2][C:24](=[O:26])[CH3:25]참가 물질
5
반응 조건
- 온도
- 0 °C
실험 절차
The compound obtained in Step E (20 mmol) is dissolved in a mixture of water/ethyl acetate (25 ml/75 ml) cooled to 0° C. Potassium carbonate (60 mmol) is added, and then acetyl chloride (26 mmol) is added dropwise to the reaction mixture. The mixture is stirred vigorously for 30 minutes at ambient temperature. The two phases are separated and the organic phase is washed with 0.1M aqueous hydrochloric acid solution and then with water. After drying over magnesium sulphate, the organic phase is evaporated under reduced pressure. The residue obtained is recrystallised from acetonitrile to yield the title product in the form of a white solid.
후처리
- customThe two phases are separated
- washthe organic phase is washed with 0.1M aqueous hydrochloric acid solution
- dry with materialAfter drying over magnesium sulphate
- customthe organic phase is evaporated under reduced pressure
- customThe residue obtained
- customis recrystallised from acetonitrile
출처 및 근거
- ORD 기록
- ord-f2bc9330ad344068a5eecf2f38f2ba1d
- 출처 데이터셋
- uspto-grants-2011_05
- 특허 번호
- US07947852B2
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