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Methanol → 8-chloro-N-[4-(ethylsulfonyl)-2-oxobutyl]dibenz[b,f][1,4]oxazepin-10(11H)-carboxamide

HRID 1769652
ノート
印刷プレビュー

反応式

HRID 1769652 の反応式
[Cl:1][C:2]1[CH:24]=[CH:23][C:5]2[O:6][C:7]3[CH:22]=[CH:21][CH:20]=[CH:19][C:8]=3[CH2:9][N:10]([C:11]([NH:13][CH2:14][C:15](=[O:18])[CH:16]=[CH2:17])=[O:12])[C:4]=2[CH:3]=1.[CH2:25]([SH:27])[CH3:26].N1CCCCC1.[OH-:34].C([N+](C)(C)C)C1C=CC=CC=1.C[OH:47]>C(Cl)Cl>[Cl:1][C:2]1[CH:24]=[CH:23][C:5]2[O:6][C:7]3[CH:22]=[CH:21][CH:20]=[CH:19][C:8]=3[CH2:9][N:10]([C:11]([NH:13][CH2:14][C:15](=[O:18])[CH2:16][CH2:17][S:27]([CH2:25][CH3:26])(=[O:47])=[O:34])=[O:12])[C:4]=2[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

7

反応物 5

HCID 887MethanolHCID 6343EthanethiolHCID 8082PiperidineHCID 66854Benzyltrimethylammonium hydroxideHCID 108311978-chloro-N-(2-oxo-3-butenyl)dibenz-[b,f][1,4]oxazepin-10(11H)-carboxamide

生成物 1

HCID 105990888-chloro-N-[4-(ethylsulfonyl)-2-oxobutyl]dibenz[b,f][1,4]oxazepin-10(11H)-carboxamide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

A solution of 8-chloro-N-(2-oxo-3-butenyl)dibenz[b,f][1,4]oxazepin-10(11H)-carboxamide (1.00 gram), ethanethiol (0.23 mL), piperidine (0.092 mL), and N-benzyltrimethylammonium hydroxide (0,092 mL) in methylene chloride (16 mL) and methanol (4 mL) was stirred at room temperature for 5 hours. The reaction was diluted with methylene chloride (100 mL), washed with 100 mL each of 1N HCl (two times), water, saturated aqueous sodium bicarbonate, and brine, dried over MgSO4, and evaporated in vacuo. The crude product was purified by flash chromatography through silica gel 60 (350 mL) using 92:8 methylene chloride: ethyl acetate to yield a colorless oil. The yield of the title compound was 0.38 gram. (32%).

後処理

  1. washwashed with 100 mL each of 1N HCl (two times), water, saturated aqueous sodium bicarbonate, and brine
  2. dry with materialdried over MgSO4
  3. customevaporated in vacuo
  4. customThe crude product was purified by flash chromatography through silica gel 60 (350 mL)
  5. customethyl acetate to yield a colorless oil

出典と根拠

ORDレコード
ord-2b5c76fc8da44789b35dde5a24f94aed
出典データセット
uspto-grants-1995_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05382578

反応ノート

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