Acetyl chloride → HCID 44359309, 화합물

HRID 551778노트

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HRID 551778 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

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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

  1. customThe two phases are separated
  2. washthe organic phase is washed with 0.1M aqueous hydrochloric acid solution
  3. dry with materialAfter drying over magnesium sulphate
  4. customthe organic phase is evaporated under reduced pressure
  5. customThe residue obtained
  6. customis recrystallised from acetonitrile

출처 및 근거

ORD 기록
ord-f2bc9330ad344068a5eecf2f38f2ba1d
출처 데이터셋
uspto-grants-2011_05
특허 번호
US07947852B2

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