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Potassium peroxymonosulphate → 2-chloro-8-(methylsulfonyl)-7H-purine

HRID 929188
ノート
印刷プレビュー

反応式

HRID 929188 の反応式
[Cl:1][C:2]1[N:10]=[C:9]2[C:5]([NH:6][C:7](SC)=[N:8]2)=[CH:4][N:3]=1.[S:13]([O-:18])(O[O-])(=O)=[O:14].[K+].[K+].[CH3:21]C#N.O>>[Cl:1][C:2]1[N:10]=[C:9]2[C:5]([NH:6][C:7]([S:13]([CH3:21])(=[O:18])=[O:14])=[N:8]2)=[CH:4][N:3]=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 3

HCID 10313463Potassium peroxymonosulphateHCID 18373917Acetonitrile--water (1/1)HCID 457896422-Chloro-8-(methylsulfanyl)-7H-purine

生成物 1

HCID 900418402-chloro-8-(methylsulfonyl)-7H-purine

実験手順

To a stirring solution of 2-chloro-8-(methylthio)-7H-purine (700.0 mg, 3.49 mmol) in 50% CH3CN/water (44.8 mL) was added potassium peroxymonosulfate (oxone, 4.72 g, 7.68 mmol). The reaction was stirred under N2 at RT for 17 h, then filtered and the filtrate was added to a stirring EtOAc (1 L)/water (0.56 L) mixture. The aqueous layer was separated and back-extracted with EtOAc (0.2 L). The combined organic layers were evaporated under reduced pressure to afford the title compound. LC-MS: calculated for C6H5ClN4O2S 231.98 observed m/e: 233.11 (M+H)+ (Rt 0.58/2.0 min).

後処理

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
  1. filtrationfiltered
  2. additionthe filtrate was added to a stirring EtOAc (1 L)/water (0.56 L) mixture
  3. customThe aqueous layer was separated
  4. extractionback-extracted with EtOAc (0.2 L)
  5. customThe combined organic layers were evaporated under reduced pressure

出典と根拠

ORDレコード
ord-ad17307b7001478ba47827fc0ed4eb03
出典データセット
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09290517B2

反応ノート

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