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m-Chloroperbenzoic acid → 2-Acetamido-1,3-diacetoxy-2-(4-octylsulfonylbenzyl)propane

HRID 862862
ノート
印刷プレビュー

反応式

HRID 862862 の反応式
[C:1]([NH:4][C:5]([CH2:16][C:17]1[CH:22]=[CH:21][C:20]([S:23]([CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH3:32])=[O:24])=[CH:19][CH:18]=1)([CH2:11][O:12][C:13](=[O:15])[CH3:14])[CH2:6][O:7][C:8](=[O:10])[CH3:9])(=[O:3])[CH3:2].ClC1C=CC=C(C(OO)=[O:41])C=1.[OH-].[Ca+2].[OH-]>C(Cl)(Cl)Cl>[C:1]([NH:4][C:5]([CH2:16][C:17]1[CH:22]=[CH:21][C:20]([S:23]([CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH3:32])(=[O:41])=[O:24])=[CH:19][CH:18]=1)([CH2:6][O:7][C:8](=[O:10])[CH3:9])[CH2:11][O:12][C:13](=[O:15])[CH3:14])(=[O:3])[CH3:2]
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 70297m-Chloroperbenzoic acidHCID 6093208Calcium HydroxideHCID 218492772-Acetamido-1,3-diacetoxy-2-(4-octylsulfinylbenzyl)propane

生成物 1

HCID 218493422-Acetamido-1,3-diacetoxy-2-(4-octylsulfonylbenzyl)propane収率 47.5%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

To a solution (10 ml) of 2-acetamido-1,3-diacetoxy-2-(4-octylsulfinylbenzyl)propane (330 mg) in chloroform was added m-chloroperbenzoic acid (244 mg) under ice-cooling. The mixture was stirred for 2.5 hours and then at room temperature for 1.5 hours. Calcium hydroxide (0.1 g) was added to the reaction mixture and the mixture was stirred at room temperature for 45 minutes. The insoluble matters were filtered off and the filtrate was concentrated under reduced pressure. The residue was recrystallized from hexane-ethyl acetate to give 162 mg of the subject compound.

後処理

  1. temperaturecooling
  2. waitat room temperature for 1.5 hours
  3. stirringthe mixture was stirred at room temperature for 45 minutes
  4. filtrationThe insoluble matters were filtered off
  5. concentrationthe filtrate was concentrated under reduced pressure
  6. customThe residue was recrystallized from hexane-ethyl acetate

出典と根拠

ORDレコード
ord-5505b5e667d847a0be6fa845705d47a2
出典データセット
uspto-grants-1998_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05719176

反応ノート

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