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

HRID 22041
ノート
印刷プレビュー

反応式

HRID 22041 の反応式
[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]
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 112011,1-DibromoethaneHCID 11430Potassium CarbonateHCID 971062Ethyl N-{[3-(trifluoromethyl)phenyl]carbamothioyl}carbamate

生成物 1

HCID 542258332-Ethoxycarbonylimino-3-(3-trifluoromethylphenyl)thiazolidine収率 83.1%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-bf1c16cb7cb041d98a3f8cccca2966a4
出典データセット
uspto-grants-1995_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05426188

反応ノート

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