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Water → 4-Nitrophenyl thiomorpholine-4-carboxylate 1-oxide

HRID 220030
ノート
印刷プレビュー

反応式

HRID 220030 の反応式
[N:1]1([C:7]([O:9][C:10]2[CH:15]=[CH:14][C:13]([N+:16]([O-:18])=[O:17])=[CH:12][CH:11]=2)=[O:8])[CH2:6][CH2:5][S:4][CH2:3][CH2:2]1.ClC1C=CC=C(C(OO)=[O:27])C=1.O>ClCCl>[N:1]1([C:7]([O:9][C:10]2[CH:11]=[CH:12][C:13]([N+:16]([O-:18])=[O:17])=[CH:14][CH:15]=2)=[O:8])[CH2:2][CH2:3][S:4](=[O:27])[CH2:5][CH2:6]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 962WaterHCID 70297m-Chloroperbenzoic acidHCID 581164954-Nitrophenyl thiomorpholine-4-carboxylate

生成物 1

HCID 581165434-Nitrophenyl thiomorpholine-4-carboxylate 1-oxide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

13.1 g (49.0 mmol) of 4-nitrophenyl thiomorpholine-4-carboxylate were initially charged in 135 ml of dichloromethane and admixed at 0° C. with 7.6 g (44.1 mmol) of m-chloroperbenzoic acid in portions. The mixture was stirred at RT for two hours, water was added and the organic phase was removed. The organic phase was washed rapidly with saturated aqueous sodium hydrogencarbonate solution, filtered and concentrated under reduced pressure. The crude product was purified by means of preparative HPLC. Yield: 7.8 g (56% of theory)

後処理

  1. customthe organic phase was removed
  2. washThe organic phase was washed rapidly with saturated aqueous sodium hydrogencarbonate solution
  3. filtrationfiltered
  4. concentrationconcentrated under reduced pressure
  5. customThe crude product was purified by means of preparative HPLC

出典と根拠

ORDレコード
ord-cb3e826cc9b44cc08b789c167fe2fcab
出典データセット
uspto-grants-2012_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08202862B2

反応ノート

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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