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Potassium Carbonate → 7-Methanesulfonyl-2,3,4,5-tetrahydro-1H-benzo[d]azepine

HRID 33204
ノート
印刷プレビュー

反応式

HRID 33204 の反応式
C([N:4]1[CH2:10][CH2:9][C:8]2[CH:11]=[CH:12][C:13]([S:15]([CH3:18])(=[O:17])=[O:16])=[CH:14][C:7]=2[CH2:6][CH2:5]1)(=O)C.C(=O)([O-])[O-].[K+].[K+]>Cl>[CH3:18][S:15]([C:13]1[CH:12]=[CH:11][C:8]2[CH2:9][CH2:10][NH:4][CH2:5][CH2:6][C:7]=2[CH:14]=1)(=[O:17])=[O:16]
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 11430Potassium CarbonateHCID 112656343-Acetyl-7-methylsulfonyl-2,3,4,5-tetrahydro-1H-3-benzazepine

生成物 1

HCID 117362667-Methanesulfonyl-2,3,4,5-tetrahydro-1H-benzo[d]azepine収率 32%

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

A solution of 3-acetyl-7-methylsulfonyl-2,3,4,5-tetrahydro-1H-3-benzazepine (1.75 g, 6.55 mmol) in 5 M hydrochloric acid was heated at reflux for 18 h. The reaction mixture was then cooled to room temperature, basified to pH=12 with potassium carbonate and the solvent evaporated in vacuo. The solid residue was then extracted with ethyl acetate (5×60 ml) and the combined organics dried (Na2SO4). The solvent was then evaporated in vacuo to give the title compound (450 mg, 32%) as a pale yellow oil.

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  1. temperatureat reflux for 18 h
  2. customthe solvent evaporated in vacuo
  3. extractionThe solid residue was then extracted with ethyl acetate (5×60 ml)
  4. dry with materialthe combined organics dried (Na2SO4)
  5. customThe solvent was then evaporated in vacuo

出典と根拠

ORDレコード
ord-baa428799dcc4f4d9fcc551287b20dc2
出典データセット
uspto-grants-2008_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07429579B2

反応ノート

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