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Triethylamine → HCID 19370295、化合物

HRID 129756
ノート
印刷プレビュー

反応式

HRID 129756 の反応式
[CH3:1][S:2](Cl)(=[O:4])=[O:3].[CH2:6]([O:8][C:9]([N:11]([CH2:13][CH2:14][OH:15])[CH3:12])=[O:10])[CH3:7].C(N(CC)CC)C>C(Cl)Cl>[CH3:1][S:2]([O:15][CH2:14][CH2:13][N:11]([C:9]([O:8][CH2:6][CH3:7])=[O:10])[CH3:12])(=[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 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 19370355ethyl N-(2-hydroxyethyl)-N-methylcarbamate

生成物 1

HCID 19370295HCID 19370295、化合物収率 103.1%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

1.65 g of methanesulfonyl chloride was added dropwise, with stirring, to a solution of 1.66 g of 2-(N-ethoxycarbonyl-N-methylamino)ethanol and 1.65 g of triethylamine in 20 ml of methylene chloride, whilst ice-cooling, and the solution was then stirred at the same temperature for 30 minutes. At the end of this time, the mixture was poured into ice-water and extracted with methylene chloride. The extracts were combined and washed with water, after which they were dried over anhydrous sodium sulfate. Evaporation of the solvent under reduced pressure gave a residue which was purified by column chromatography through silica gel, using a 2:1 by volume mixture of ethyl acetate and hexane as the eluent, to give 2.62 g (yield 81%) of the title compound as an oil.

後処理

  1. temperaturecooling
  2. extractionextracted with methylene chloride
  3. washwashed with water
  4. dry with materialafter which they were dried over anhydrous sodium sulfate
  5. customEvaporation of the solvent under reduced pressure
  6. customgave a residue which
  7. customwas purified by column chromatography through silica gel
  8. additionby volume mixture of ethyl acetate and hexane as the eluent

出典と根拠

ORDレコード
ord-d7fbf0c63ccd48629c71ca48031e669e
出典データセット
uspto-grants-1995_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05470851

反応ノート

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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