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Hydrazine hydrate (1:1) → HCID 86757406、化合物

HRID 1596756
ノート
印刷プレビュー

反応式

HRID 1596756 の反応式
[CH2:1]([N:8]1[CH2:16][C:15]2([C:17]([O:19][CH3:20])=[O:18])[CH:10]([C:11](=O)[CH2:12][CH2:13][CH:14]2[C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.O.[NH2:29][NH2:30]>C(O)C>[CH2:1]([N:8]1[CH2:16][C:15]2([C:17]([O:19][CH3:20])=[O:18])[CH:10]([C:11](=[N:29][NH2:30])[CH2:12][CH2:13][CH:14]2[C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 11302988methyl(3aRS,4SR,7aRS)-2-benzyl-7-oxo-4-phenyloctahydroisoindole-3a-carboxylate

生成物 1

HCID 86757406HCID 86757406、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of 100 g (0.275 mol) of the levorotatory enantiomer of methyl (3aRS,4RS,7aSR)-2-benzyl-4-phenyl-7-oxoperhydroisoindole-3a-carboxylate and of 50 g (1 mol) of hydrazine hydrate in 750 cm3 of ethanol is brought to reflux for one and a half hours. After concentrating the ethanol under reduced pressure, the residue is taken up in 400 cm3 of dichloromethane and the organic phase is washed with distilled water and then with a saturated aqueous sodium chloride solution, dried over magnesium sulfate and concentrated under reduced pressure. 100 g (960%) of the levorotatory enantiomer of methyl (3aRS,4SR,7aRS)-2-benzyl-7-hydrazono-4-phenylperhydroisoindole-3a-carboxylate are thus obtained in the form of a yellow oil used as is in the following stage.

後処理

  1. temperatureto reflux for one and a half hours
  2. concentrationAfter concentrating the ethanol under reduced pressure
  3. washthe organic phase is washed with distilled water
  4. dry with materialwith a saturated aqueous sodium chloride solution, dried over magnesium sulfate
  5. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-96ce0a1a56174f96b5067abbb0d893d4
出典データセット
uspto-grants-2001_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06291679B1

反応ノート

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