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Triethylamine → 3-(tert-Butyloxycarbonyl)-7-methanesulfonyloxy-2,3,4,5tetrahydro-1H-3-benzazepine

HRID 33212
ノート
印刷プレビュー

反応式

HRID 33212 の反応式
[C:1]([O:5][C:6]([N:8]1[CH2:14][CH2:13][C:12]2[CH:15]=[CH:16][C:17]([OH:19])=[CH:18][C:11]=2[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[CH3:20][S:21](Cl)(=[O:23])=[O:22].C(N(CC)CC)C>ClCCl>[C:1]([O:5][C:6]([N:8]1[CH2:14][CH2:13][C:12]2[CH:15]=[CH:16][C:17]([O:19][S:21]([CH3:20])(=[O:23])=[O:22])=[CH:18][C:11]=2[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:2])[CH3:3]
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 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 18173274tert-butyl 7-hydroxy-2,3,4,5-tetrahydro-1H-3-benzazepine-3-carboxylate

生成物 1

HCID 112792893-(tert-Butyloxycarbonyl)-7-methanesulfonyloxy-2,3,4,5tetrahydro-1H-3-benzazepine収率 102.5%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A solution of 3-(tert-butyloxycarbonyl)-7-hydroxy-2,3,4,5-tetrahydro-1H-3-benzazepine (3.0 g, 0.011 mol), methanesulfonylchloride (1.44 g, 0.013 mol), triethylamine (1.27 g, 0.013 mol) and dichloromethane (50 ml) was stirred at room temperature for 18 h. The reaction mixture was then partitioned between dichloromethane (50 ml) and a saturated solution of sodium hydrogen carbonate (50 ml). The organic layer was separated, washed with water (50 ml) and then dried (Na2SO4). The solvent was then evaporated in vacuo to give the title compound (3.85 g, 99%) as a pale yellow oil.

後処理

  1. customThe reaction mixture was then partitioned between dichloromethane (50 ml)
  2. customThe organic layer was separated
  3. washwashed with water (50 ml)
  4. dry with materialdried (Na2SO4)
  5. customThe solvent was then evaporated in vacuo

出典と根拠

ORDレコード
ord-cb9607fd695f4594a7900c83431f560f
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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