Hydrazine hydrate (1:1) → 3(R)-amino-2,3-dihydro-1,5(5H)-benzothiazepin-4-one

HRID 980619노트

반응식

HRID 980619 반응식
C1(=O)[N:5]([C@@H:6]2[C:12](=[O:13])[NH:11][C:10]3[CH:14]=[CH:15][CH:16]=[CH:17][C:9]=3[S:8][CH2:7]2)C(=O)C2=CC=CC=C12.O.NN>C(O)C>[NH2:5][C@@H:6]1[C:12](=[O:13])[NH:11][C:10]2[CH:14]=[CH:15][CH:16]=[CH:17][C:9]=2[S:8][CH2:7]1

참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 134546823(R)-phthalimido-2,3-dihydro-1,5(5H)-benzothiazepin-4-one

생성물 1

HCID 133751443(R)-amino-2,3-dihydro-1,5(5H)-benzothiazepin-4-one수율 62.6%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 3(R)-phthalimido-2,3-dihydro-1,5-(5H)-benzothiazepin-4-one (10 g), ethanol (500 ml) and hydrazine hydrate (6.2 g) is refluxed for 1 hour. After ethanol is removed by evaporation under reduced pressure, water (300 ml) is added, and the mixture is extracted with ethyl acetate (400 ml). The extract is washed with 0.1 N sodium hydroxide solution (100 ml×2) and water (100 ml) successively, dried over anhydrous magnesium sulfate and concentrated in vacuo to give 3(R)-amino-2,3-dihydro-1,5(5H)-benzothiazepin-4-one (3.75 g) as colorless leaflets.

후처리

  1. temperatureis refluxed for 1 hour
  2. customAfter ethanol is removed by evaporation under reduced pressure, water (300 ml)
  3. additionis added
  4. extractionthe mixture is extracted with ethyl acetate (400 ml)
  5. washThe extract is washed with 0.1 N sodium hydroxide solution (100 ml×2) and water (100 ml) successively
  6. dry with materialdried over anhydrous magnesium sulfate
  7. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-5669b029bd6242e098e53a92bcc03d4c
출처 데이터셋
uspto-grants-1987_01
특허 번호
US04638000

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