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三乙胺 → 2-(Methanesulfonyloxymethyl)-6-methyl-nitrobenzene

HRID 1069476
笔记
打印预览

反应方程式

HRID 1069476 反应方程式
[CH3:1][S:2](Cl)(=[O:4])=[O:3].[CH3:6][C:7]1[C:8]([N+:15]([O-:17])=[O:16])=[C:9]([CH:12]=[CH:13][CH:14]=1)[CH2:10][OH:11].C(N(CC)CC)C>C(Cl)Cl>[CH3:1][S:2]([O:11][CH2:10][C:9]1[CH:12]=[CH:13][CH:14]=[C:7]([CH3:6])[C:8]=1[N+:15]([O-:17])=[O:16])(=[O:4])=[O:3]
参与物实验过程后处理来源与证据反应笔记

参与物

5

反应物 3

HCID 8471三乙胺HCID 31297甲基磺酰氯HCID 5619893-甲基-2-硝基苄醇

产物 1

HCID 157669562-(Methanesulfonyloxymethyl)-6-methyl-nitrobenzene收率 97.9%

试剂、催化剂与溶剂 1

HCID 6344二氯甲烷溶剂2 次

实验过程

At 10-15° C., 27 g (0.23 mol) of methanesulfonyl chloride dissolved in 20 ml of CH2Cl2 is dripped into a mixture of 34 g (0.2 mol) of 3-methyl-2-nitrobenzyl alcohol and 27 g (0.27 mol) of triethylamine in 100 ml of CH2Cl2. The reaction mixture is stirred for 1 hour at room temperature and is then extracted with water. The organic phase is dried over MgSO4 and evaporated down. There is obtained as residue 48 g of the title compound as a yellow oil, containing about 10% of the corresponding benzyl chloride as impurity. The crude product is used for the next reaction without any further purification.

后处理

  1. extractionis then extracted with water
  2. dry with materialThe organic phase is dried over MgSO4
  3. customevaporated down

来源与证据

ORD记录
ord-10634ab235344e1d8cb90a9a5c93b753
来源数据集
uspto-grants-2001_06
DOI
10.6084/m9.figshare.5104873.v1
专利号
US06252083B1

反应笔记

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本页导航参与物实验过程后处理来源与证据反应笔记