Hydrazine hydrate (1:1) → 3-Amino-2,3,4,5-tetrahydro-2-oxo-1H-1-benzazepin-1-t-butyl acetate

HRID 1031816ノート

反応式

HRID 1031816 の反応式
[O:1]=[C:2]1[CH:8]([N:9]2C(=O)C3=CC=CC=C3C2=O)[CH2:7][CH2:6][C:5]2[CH:20]=[CH:21][CH:22]=[CH:23][C:4]=2[N:3]1[CH2:24][C:25]([O:27][C:28]([CH3:31])([CH3:30])[CH3:29])=[O:26].O.NN>C(O)C>[NH2:9][CH:8]1[CH2:7][CH2:6][C:5]2[CH:20]=[CH:21][CH:22]=[CH:23][C:4]=2[N:3]([CH2:24][C:25]([O:27][C:28]([CH3:30])([CH3:29])[CH3:31])=[O:26])[C:2]1=[O:1]

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 14010679tert-butyl 2-oxo-3-phthalimido-2,3,4,5-tetrahydro-1H-1-benzazepine-1-acetate

生成物 1

HCID 36741653-Amino-2,3,4,5-tetrahydro-2-oxo-1H-1-benzazepin-1-t-butyl acetate収率 86.9%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To 100 ml of ethanol is added 10 g of tert-butyl 2-oxo-3-phthalimido-2,3,4,5-tetrahydro-1H-1-benzazepine-1-acetate, and 5 g of hydrazine hydrate is added to the mixture, followed by refluxing for 2 hours. The reaction mixture is concentrated under reduced pressure, and 300 ml of water is added to the residue, followed by extraction with 200 ml of ethyl acetate. The extract is washed with 1N aqueous sodium hydroxide and water, successively, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The crystals, which separate out, are treated with a mixture of ether and petroleum ether and collected by filtration to give 6 g of tert-butyl 3-amino-2-oxo-2,3,4,5-tetrahydro-1H-1-benzazepine-1-acetate as colorless prisms. m.p. 121°-122° C.

後処理

  1. additionis added to the mixture
  2. temperatureby refluxing for 2 hours
  3. concentrationThe reaction mixture is concentrated under reduced pressure, and 300 ml of water
  4. additionis added to the residue
  5. extractionfollowed by extraction with 200 ml of ethyl acetate
  6. washThe extract is washed with 1N aqueous sodium hydroxide and water
  7. dry with materialsuccessively, dried over anhydrous magnesium sulfate
  8. concentrationconcentrated under reduced pressure
  9. customThe crystals, which separate out
  10. additionare treated with a mixture of ether and petroleum ether
  11. filtrationcollected by filtration

出典と根拠

ORDレコード
ord-c2556416069d4324aed7596a711495ad
出典データセット
uspto-grants-1990_09
特許番号
US04954625

反応ノート

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