Methylamine → ([2-(Methylamino)ethyl]sulfonyl)benzene

HRID 745169

反応式

HRID 745169 の反応式
Cl[CH2:2][CH2:3][S:4]([C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)(=[O:6])=[O:5].[CH3:13][NH2:14]>C(#N)C>[CH3:13][NH:14][CH2:2][CH2:3][S:4]([C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)(=[O:6])=[O:5]

参加物

4

反応物 2

HCID 6329MethylamineHCID 13646((2-Chloroethyl)sulphonyl)benzene

生成物 1

HCID 5152138([2-(Methylamino)ethyl]sulfonyl)benzene

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

A solution of 2-chloroethylphenyl sulfone and a large excess of methylamine (40% solution in water) in acetonitrile is stirred at room temperature overnight. The solvent is removed in vacuo and the residue is partitioned between methylene chloride and dilute sodium hydroxide. The methylene chloride solution is extracted with dilute sulfuric acid. The acidic extract is made basic with 50% sodium hydroxide and the basic solution is extracted with methylene chloride. The methylene chloride solution is dried over magnesium sulfate and the solvent is removed in vacuo to give the title compound.

後処理

  1. customThe solvent is removed in vacuo
  2. customthe residue is partitioned between methylene chloride and dilute sodium hydroxide
  3. extractionThe methylene chloride solution is extracted with dilute sulfuric acid
  4. extractionThe acidic extract
  5. extractionthe basic solution is extracted with methylene chloride
  6. dry with materialThe methylene chloride solution is dried over magnesium sulfate
  7. customthe solvent is removed in vacuo

出典と根拠

ORDレコード
ord-4bcb9985990d4f0a9ba58e9444d206e9
出典データセット
uspto-grants-1986_07
特許番号
US04597902

関連ノート

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