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Hydrazine → HCID 66975547、化合物

HRID 1022592
ノート
印刷プレビュー

反応式

HRID 1022592 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([C:9]2([CH2:23][N:24]3C(=O)C4C(=CC=CC=4)C3=O)[O:15][CH2:14][CH2:13][N:12]([C:16]([O:18][C:19]([CH3:22])([CH3:21])[CH3:20])=[O:17])[CH2:11][CH2:10]2)[CH:5]=[CH:6][C:7]=1[Cl:8].NN>C(O)C>[NH2:24][CH2:23][C:9]1([C:4]2[CH:5]=[CH:6][C:7]([Cl:8])=[C:2]([Cl:1])[CH:3]=2)[O:15][CH2:14][CH2:13][N:12]([C:16]([O:18][C:19]([CH3:22])([CH3:21])[CH3:20])=[O:17])[CH2:11][CH2:10]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 9321HydrazineHCID 66975369HCID 66975369、化合物

生成物 1

HCID 66975547HCID 66975547、化合物収率 87.2%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution of tert-butyl (7RS)-7-(3,4-dichlorophenyl)-7-[(1,3-dioxo-1,3-dihydro-2H-isoindol-2-yl)methyl]-1,4-oxazepane-4-carboxylate (1.39 g) in ethanol (14 ml) was added hydrazine (2.8 ml), and the mixture was stirred at room temperature for 14 hr. The precipitate was removed by filtration, and the solvent of the filtrate was evaporated under reduced pressure. Water was added to the residue, and the mixture was extracted with ethyl acetate. The obtained extract was washed with water and brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure to give the title compound (0.9 g).

後処理

  1. customThe precipitate was removed by filtration
  2. customthe solvent of the filtrate was evaporated under reduced pressure
  3. additionWater was added to the residue
  4. extractionthe mixture was extracted with ethyl acetate
  5. extractionThe obtained extract
  6. washwas washed with water and brine
  7. dry with materialdried over anhydrous magnesium sulfate
  8. customThe solvent was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-acef3fe8aad74fe68e1c5099a3d2ad96
出典データセット
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08722662B2

反応ノート

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