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

HRID 980619ノート

反応式

HRID 980619 の反応式
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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-5669b029bd6242e098e53a92bcc03d4c
出典データセット
uspto-grants-1987_01
特許番号
US04638000

反応ノート

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