Sodium Acetate → 3-acetyl-7-methoxy-2,3,4,5-tetrahydro-1H-3-benzazepine

HRID 542721노트

반응식

HRID 542721 반응식
Cl.[CH3:2][O:3][C:4]1[CH:14]=[CH:13][C:7]2[CH2:8][CH2:9][NH:10][CH2:11][CH2:12][C:6]=2[CH:5]=1.[C:15]([O-])(=[O:17])[CH3:16].[Na+]>C(OC(=O)C)(=O)C>[C:15]([N:10]1[CH2:9][CH2:8][C:7]2[CH:13]=[CH:14][C:4]([O:3][CH3:2])=[CH:5][C:6]=2[CH2:12][CH2:11]1)(=[O:17])[CH3:16]

참가 물질

4

반응물 2

HCID 517045Sodium AcetateHCID 212429067-methoxy-2,3,4,5-tetrahydro-1H-3-benzazepine hydrochloride

생성물 1

HCID 138533493-acetyl-7-methoxy-2,3,4,5-tetrahydro-1H-3-benzazepine

시약·촉매·용매 1

HCID 7918Acetic Anhydride용매

실험 절차

A mixture of 7-methoxy-2,3,4,5-tetrahydro-1H-3-benzazepine hydrochloride (4.3 g, 0.02 m) and sodium acetate (3.3 g, 0.04 m) in acetic anhydride (13 ml) was refluxed and stirred for 16 hours, concentrated in vacuo and partitioned between methylene chloride and water. The organic phase was dried with magnesium sulfate, filtered and concentrated in vacuo to give 3-acetyl-7-methoxy-2,3,4,5-tetrahydro-1H-3-benzazepine, m.p. 89°-90°.

후처리

  1. temperaturewas refluxed
  2. concentrationconcentrated in vacuo
  3. custompartitioned between methylene chloride and water
  4. dry with materialThe organic phase was dried with magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-c081516339d44421813e9ed4b012269d
출처 데이터셋
uspto-grants-1987_04
특허 번호
US04659706

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