Benzene, 1-chloro-3-isocyanato- → N-(3-chlorophenyl)-N'-(2-chloroethyl)imidazolidinone

HRID 235989

반응식

HRID 235989 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([N:8]=[C:9]=[O:10])[CH:5]=[CH:6][CH:7]=1.[Cl:11][CH2:12][CH2:13][N:14]1[CH2:18][CH2:17]OC1=O>ClCCl.[Al+3].[Cl-].[Cl-].[Cl-]>[Cl:1][C:2]1[CH:3]=[C:4]([N:8]2[CH2:17][CH2:18][N:14]([CH2:13][CH2:12][Cl:11])[C:9]2=[O:10])[CH:5]=[CH:6][CH:7]=1

참가 물질

5

반응물 2

HCID 17968Benzene, 1-chloro-3-isocyanato-HCID 756333-(2-Chloroethyl)-1,3-oxazolidin-2-one

생성물 1

HCID 13824503N-(3-chlorophenyl)-N'-(2-chloroethyl)imidazolidinone수율 78.7%

시약·촉매·용매 2

HCID 6451240Aluminum(III) Chloride촉매HCID 6344Dichloromethane용매

반응 조건

온도
195 °C

실험 절차

A mixture of 3-chlorophenyl isocyanate (7.65 g, 50 mmoles), N-(2-chloroethyl)-2-oxazolidinone (7.5 g, 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 10.2 g (78.4 percent) of the desired product, m.p. 64° C.

후처리

  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

출처 및 근거

ORD 기록
ord-94979adb2c224e2eab50346924169805
출처 데이터셋
uspto-grants-1987_02
특허 번호
US04642351

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