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Water → 4,4-Dimethyl-1-[2-(methylsulfonyl)benzyl]-2-(adamantan-2-yl)-1,2-diazetidin-3-one

HRID 888853
ノート
印刷プレビュー

反応式

HRID 888853 の反応式
[CH3:1][C:2]1([CH3:26])[N:5]([CH2:6][C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=2[S:13][CH3:14])[N:4]([CH:15]2[CH:22]3[CH2:23][CH:18]4[CH2:19][CH:20]([CH2:24][CH:16]2[CH2:17]4)[CH2:21]3)[C:3]1=[O:25].[OH2:27].[OH:28]O.O>CO.[Cl-].[Cl-].[Cl-].[Cl-].[Cl-].[Ta+5]>[CH3:1][C:2]1([CH3:26])[N:5]([CH2:6][C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=2[S:13]([CH3:14])(=[O:28])=[O:27])[N:4]([CH:15]2[CH:16]3[CH2:17][CH:18]4[CH2:19][CH:20]([CH2:21][CH:22]2[CH2:23]4)[CH2:24]3)[C:3]1=[O:25]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 962WaterHCID 449047Hydrogen peroxide waterHCID 673027144,4-Dimethyl-1-[2-(methylthio)benzyl]-2-(adamantan-2-yl)-1,2-diazetidin-3-one

生成物 1

HCID 461959234,4-Dimethyl-1-[2-(methylsulfonyl)benzyl]-2-(adamantan-2-yl)-1,2-diazetidin-3-one収率 32.1%

試薬・触媒・溶媒 2

HCID 10269745Tantalum chloride触媒
HCID 887
Methanol
溶媒

実験手順

A solution of 4,4-dimethyl-1-[2-(methylthio)benzyl]-2-(adamantan-2-yl)-1,2-diazetidin-3-one (7.20 mg, 0.0186 mmol) prepared in Example 60 in methanol was added sequentially with tantalum pentachloride (3.30 mg, 0.00930 mmol) and hydrogen peroxide water (5.70 mg, 0.0558 mmol) at room temperature, and the resultant was stirred at the same temperature for 36.5 hours. The reaction solution was added with water and extracted with diethyl ether. The organic layer was dried over anhydrous sodium sulfate and concentrated in vacuo. The obtained residue was purified using Preparative Thin-Layer chromatography (hexane:ethyl acetate=1:5), and the title compound (2.40 mg, 32.0%) was obtained as a white crystalline powder.

後処理

  1. extractionextracted with diethyl ether
  2. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  3. concentrationconcentrated in vacuo
  4. customThe obtained residue was purified

出典と根拠

ORDレコード
ord-cf646f32ff62497483ef5d8ec9c5e2d6
出典データセット
uspto-grants-2012_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08252781B2

反応ノート

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