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Methanesulfonyl chloride → 2-[N-(4-Methanesulphonamidobenzyl)-N-methylamino]-5-methanesulphonamidoindane

HRID 1761873
ノート
印刷プレビュー

反応式

HRID 1761873 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 31297Methanesulfonyl chlorideHCID 150232235-Amino-2-[N-(4-aminobenzyl)-N-methylamino]indane

生成物 1

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

試薬・触媒・溶媒 2

HCID 1049Pyridine溶媒HCID 6212Chloroform溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-9652492b00294be1a172c2e304feac5b
出典データセット
uspto-grants-1989_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04829071

反応ノート

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