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Divinyl sulfone → 4-Benzylthiomorpholine 1,1-Dioxide

HRID 433949
ノート
印刷プレビュー

反応式

HRID 433949 の反応式
[CH:1]([S:3]([CH:6]=[CH2:7])(=[O:5])=[O:4])=[CH2:2].[CH2:8]([NH2:15])[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1>C(O)C>[CH2:8]([N:15]1[CH2:7][CH2:6][S:3](=[O:5])(=[O:4])[CH2:1][CH2:2]1)[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH: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 6496Divinyl sulfoneHCID 7504Benzylamine

生成物 1

HCID 3184544-Benzylthiomorpholine 1,1-Dioxide収率 39.9%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Divinyl sulphone (0.8 ml, 10 mmol) was added to a solution of benzylamine (1.09 ml, 10 mmol) in ethanol (4 ml) and heated under reflux for 2 hours. The solvent was removed under reduced pressure, the residue dissolved in dichloromethane (30 ml) and washed with saturated aqueous sodium hydrogencarbonate solution (15 ml), dried over MgSO4, filtered and concentrated under reduced pressure. The residue was purified by column chromatography on silica gel eluting with a gradient system of dichloromethane:methanol (100:0 to 99:1) to afford the title compound as a yellow oil (0.9 g).

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. temperatureheated
  2. temperatureunder reflux for 2 hours
  3. customThe solvent was removed under reduced pressure
  4. dissolutionthe residue dissolved in dichloromethane (30 ml)
  5. washwashed with saturated aqueous sodium hydrogencarbonate solution (15 ml)
  6. dry with materialdried over MgSO4
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure
  9. customThe residue was purified by column chromatography on silica gel eluting with a gradient system of dichloromethane:methanol (100:0 to 99:1)

出典と根拠

ORDレコード
ord-1b06437c69b447bea9aea42d002cdbf0
出典データセット
uspto-grants-2003_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06670366B1

反応ノート

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