1,1-Dibromoethane → 2-Ethoxycarbonylimino-3-(3-trifluoromethylphenyl)thiazolidine

HRID 5327

반응식

HRID 5327 반응식
[F:1][C:2]([F:19])([F:18])[C:3]1[CH:4]=[C:5]([NH:9][C:10]([NH:12][C:13]([O:15][CH2:16][CH3:17])=[O:14])=[S:11])[CH:6]=[CH:7][CH:8]=1.Br[CH:21](Br)[CH3:22].C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[CH2:16]([O:15][C:13]([N:12]=[C:10]1[N:9]([C:5]2[CH:6]=[CH:7][CH:8]=[C:3]([C:2]([F:18])([F:1])[F:19])[CH:4]=2)[CH2:22][CH2:21][S:11]1)=[O:14])[CH3:17]

참가 물질

5

반응물 3

HCID 112011,1-DibromoethaneHCID 11430Potassium CarbonateHCID 971062Ethyl N-{[3-(trifluoromethyl)phenyl]carbamothioyl}carbamate

생성물 1

HCID 542258332-Ethoxycarbonylimino-3-(3-trifluoromethylphenyl)thiazolidine수율 83.1%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

A solution of N-(3-trifluoromethylphenyl)-N'-ethoxycarbonylthiourea (1.8 g), dibromoethane (1.29 g) and anhydrous potassium carbonate (2.6 g) in acetone (20 ml) was refluxed for 5 hours. The solvent was removed by distillation, and the residue was extracted with diethyl ether. The extract was washed with water, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was recrystallized from a mixture of hexane and ethanol to give 1.63 g of 2-ethoxycarbonylimino-3-(3-trifluoromethylphenyl)thiazolidine. m.p., 75.8° C.

후처리

  1. customThe solvent was removed by distillation
  2. extractionthe residue was extracted with diethyl ether
  3. washThe extract was washed with water
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was recrystallized from a mixture of hexane and ethanol

출처 및 근거

ORD 기록
ord-fa8d09f785da43d08f3fafc57bc6778e
출처 데이터셋
uspto-grants-1993_09
특허 번호
US05244863

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