Ethanol → Bis(4-n-pentylcyclohexylsulfonyl)diazomethane

HRID 51187

反応式

HRID 51187 の反応式
[CH2:1]([CH:6]1[CH2:11][CH2:10][CH:9]([S:12]([CH2:15][S:16]([CH:19]2[CH2:24][CH2:23][CH:22]([CH2:25][CH2:26][CH2:27][CH2:28][CH3:29])[CH2:21][CH2:20]2)(=[O:18])=[O:17])(=[O:14])=[O:13])[CH2:8][CH2:7]1)[CH2:2][CH2:3][CH2:4][CH3:5].C1(C)C=CC(S([N:39]=[N+:40]=[N-])(=O)=O)=CC=1.C(O)C.[OH-].[Na+]>CN(C)C=O.O>[CH2:1]([CH:6]1[CH2:7][CH2:8][CH:9]([S:12]([C:15]([S:16]([CH:19]2[CH2:20][CH2:21][CH:22]([CH2:25][CH2:26][CH2:27][CH2:28][CH3:29])[CH2:23][CH2:24]2)(=[O:18])=[O:17])=[N+:39]=[N-:40])(=[O:14])=[O:13])[CH2:10][CH2:11]1)[CH2:2][CH2:3][CH2:4][CH3:5]

参加物

7

反応物 4

HCID 702EthanolHCID 13661p-Toluenesulfonyl azideHCID 14798Sodium HydroxideHCID 22737685Bis(4-n-pentylcyclohexylsulfonyl)methane

生成物 1

HCID 22737629Bis(4-n-pentylcyclohexylsulfonyl)diazomethane収率 46%

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回HCID 6228Dimethylformamide溶媒

実験手順

In 22.4 g of dimethylformamide were dissolved 22.5 g (0.050 mol) of the bis(4-n-pentylcyclohexylsulfonyl)methane prepared above and 14.8 g (0.075 mol) of p-toluenesulfonylazide. To this solution were added 90.1 g of ethanol and 22.2 g of water. The solution was cooled on an ice bath, to which 2.0 g (0.050 mol) of sodium hydroxide in 23 g of water was added dropwise at a temperature below 5° C. The solution was ripened at the temperature for 6.5 hours. Filtration of the crystals gave 2.6 g of the desired bis(4-n-pentylcyclohexylsulfonyl)diazomethane. The yield was 46%.

後処理

  1. additionwas added dropwise at a temperature below 5° C
  2. filtrationFiltration of the crystals

出典と根拠

ORDレコード
ord-7eaa13038eb44482a5d299dd3d4e07c0
出典データセット
uspto-grants-2004_03
特許番号
US06713612B2

関連ノート

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