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甲基磺酰氯 → 2-[N-(4-Methanesulphonamidobenzyl)-N-methylamino]-5-methanesulphonamidoindane

HRID 1761873
笔记
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反应方程式

HRID 1761873 反应方程式
[CH3:1][S:2](Cl)(=[O:4])=[O:3].[NH2:6][C:7]1[CH:8]=[C:9]2[C:13](=[CH:14][CH:15]=1)[CH2:12][CH:11]([N:16]([CH2:18][C:19]1[CH:24]=[CH:23][C:22]([NH2:25])=[CH:21][CH:20]=1)[CH3:17])[CH2:10]2>N1C=CC=CC=1.C(Cl)(Cl)Cl>[CH3:1][S:2]([NH:6][C:7]1[CH:8]=[C:9]2[C:13](=[CH:14][CH:15]=1)[CH2:12][CH:11]([N:16]([CH2:18][C:19]1[CH:20]=[CH:21][C:22]([NH:25][S:2]([CH3:1])(=[O:4])=[O:3])=[CH:23][CH:24]=1)[CH3:17])[CH2:10]2)(=[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 2

HCID 31297甲基磺酰氯HCID 150232235-Amino-2-[N-(4-aminobenzyl)-N-methylamino]indane

产物 1

HCID 150149922-[N-(4-Methanesulphonamidobenzyl)-N-methylamino]-5-methanesulphonamidoindane

试剂、催化剂与溶剂 2

HCID 1049吡啶溶剂HCID 6212三氯甲烷溶剂

实验过程

Methanesulphonyl chloride (0.53 ml) was added to 5-amino-2-[N-(4-aminobenzyl)-N-methylamino]indane (1.1 g) in pyridine and the reaction mixture was stirred at room temperature for 17 hours. The solvent was then removed by evaporation in vacuo and the residue taken up in methylene chloride, washed with aqueous sodium bicarbonate, dried (MgSO4) and evaporated in vacuo. The resulting gum was purified by column chromatography on silica eluting with methylene chloride containing methanol (0% up to 2%). The product-containing fractions were combined and evaporated to dryness in vacuo to give a colourless foam. This foam was dissolved in chloroform and the solution was evaporated to dryness in vacuo to give the title compound as a colourless foam, yield 0.2 g.

后处理

  1. customThe solvent was then removed by evaporation in vacuo
  2. washwashed with aqueous sodium bicarbonate
  3. dry with materialdried (MgSO4)
  4. customevaporated in vacuo
  5. customThe resulting gum was purified by column chromatography on silica eluting with methylene chloride
  6. additioncontaining methanol (0% up to 2%)
  7. customevaporated to dryness in vacuo
  8. customto give a colourless foam
  9. customthe solution was evaporated to dryness in vacuo

来源与证据

ORD记录
ord-9652492b00294be1a172c2e304feac5b
来源数据集
uspto-grants-1989_05
DOI
10.6084/m9.figshare.5104873.v1
专利号
US04829071

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