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Sodium Thiosulfate → 8-chlorodibenz[b,f][1,4]oxazepine-10(11H)-carboxylic acid, 2-[(phenylsulfonyl)acetyl]hydrazide

HRID 246818
ノート
印刷プレビュー

反応式

HRID 246818 の反応式
C1(S[CH2:8][C:9]([NH:11][NH:12][C:13]([N:15]2[CH2:21][C:20]3[CH:22]=[CH:23][CH:24]=[CH:25][C:19]=3[O:18][C:17]3[CH:26]=[CH:27][C:28]([Cl:30])=[CH:29][C:16]2=3)=[O:14])=[O:10])C=CC=CC=1.Cl[C:32]1[CH:33]=[C:34]([CH:39]=[CH:40][CH:41]=1)C(OO)=O.[S:42]([O-:46])([O-])(=[O:44])=S.[Na+].[Na+]>ClCCl>[C:32]1([S:42]([CH2:8][C:9]([NH:11][NH:12][C:13]([N:15]2[CH2:21][C:20]3[CH:22]=[CH:23][CH:24]=[CH:25][C:19]=3[O:18][C:17]3[CH:26]=[CH:27][C:28]([Cl:30])=[CH:29][C:16]2=3)=[O:14])=[O:10])(=[O:46])=[O:44])[CH:33]=[CH:34][CH:39]=[CH:40][CH:41]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 24477Sodium ThiosulfateHCID 70297m-Chloroperbenzoic acidHCID 139213678-chlorodibenz[b,f][1,4]oxazepine-10(11H)-carboxylic acid, 2-[(phenylthio)acetyl]hydrazide

生成物 1

HCID 139213688-chlorodibenz[b,f][1,4]oxazepine-10(11H)-carboxylic acid, 2-[(phenylsulfonyl)acetyl]hydrazide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a stirred solution of 2.0 g (4.5 mmole) of the title product of Example 2 in 40 ml of cold (ca. 0° ) dichloromethane was added 1.94 g (9.1 mmole) of 81% m-chloroperoxybenzoic acid. After about ninety minutes, 10 ml of saturated aqueous sodium thiosulfate was added. The mixture was washed sequentially with three portions of saturated aqueous sodium bicarbonate and three portions of water. The organic phase was dried over sodium sulfate, filtered, and concentrated in vacuo to give the title compound, m.p. 180°-183°.

後処理

  1. waitAfter about ninety minutes
  2. washThe mixture was washed sequentially with three portions of saturated aqueous sodium bicarbonate and three portions of water
  3. dry with materialThe organic phase was dried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-1183ab9a9abe406ba5a5e4d98980d3f9
出典データセット
uspto-grants-1987_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04704386

反応ノート

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