Cyclohexyl isocyanate → N-(cyclohexyl)-N'-(2-chloroethyl)imidazolidinone

HRID 235990

反応式

HRID 235990 の反応式
[CH:1]1([N:7]=[C:8]=[O:9])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[Cl:10][CH2:11][CH2:12][N:13]1[CH2:17][CH2:16]OC1=O.[Al+3].[Cl-].[Cl-].[Cl-]>ClCCl>[CH:1]1([N:7]2[CH2:16][CH2:17][N:13]([CH2:12][CH2:11][Cl:10])[C:8]2=[O:9])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1

参加物

5

反応物 3

HCID 18502Cyclohexyl isocyanateHCID 756333-(2-Chloroethyl)-1,3-oxazolidin-2-oneHCID 6451240Aluminum(III) Chloride

生成物 1

HCID 13824504N-(cyclohexyl)-N'-(2-chloroethyl)imidazolidinone収率 50%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
195 °C

実験手順

A mixture of cyclohexyl isocyanate (50 mmoles), N-(2-chloroethyl)-2-oxazolidinone (50 mmoles) and anhydrous AlCl3 (40 mg, 0.3 mmole) is heated at 195° C. for 6 hours with stirring. The reaction mixture is dissolved in dichloromethane and the resulting solution is washed with water twice. The dichloromethane solution is dried and evaporated and the residue distilled at reduced pressure. The distillate is recrystallized from hot hexane to give a 50 percent yield of the desired product, m.p. 60° C.-64° C.

後処理

  1. washthe resulting solution is washed with water twice
  2. dry with materialThe dichloromethane solution is dried
  3. customevaporated
  4. distillationthe residue distilled at reduced pressure
  5. customThe distillate is recrystallized from hot hexane

出典と根拠

ORDレコード
ord-f87341538a644f02b389ec24f511ea04
出典データセット
uspto-grants-1987_02
特許番号
US04642351

関連ノート

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