Tributylstannane → 1-Bromo-2-(2,2,2-trifluoroethyl)benzene

HRID 1094811노트

반응식

HRID 1094811 반응식
[Br:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[CH:8](OC(N1C=CN=C1)=S)[C:9]([F:12])([F:11])[F:10].C([SnH](CCCC)CCCC)CCC>C1(C)C=CC=CC=1>[Br:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[CH2:8][C:9]([F:10])([F:11])[F:12]

참가 물질

4

반응물 2

HCID 5948TributylstannaneHCID 57582364Imidazole-1-carbothioic acid O-[1-(2-bromophenyl)-2,2,2-trifluoroethyl]-ester

생성물 1

HCID 457904731-Bromo-2-(2,2,2-trifluoroethyl)benzene수율 96.4%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A solution of imidazole-1-carbothioic acid O-[1-(2-bromophenyl)-2,2,2-trifluoroethyl]-ester (Preparation 56, 27.0 g, 73.8 mmol) in toluene (400 ml) was heated at reflux and treated with tri-n-butyltin hydride in three portions: 22 g (75.6 mmol) at first, an additional 10 g (34.4 mmol) after 30 min, and finally 11 g (37.8 mmol) 30 min later. After the addition, the mixture was heated at reflux for another 30 min. The reaction mixture was cooled then the product was distilled at 25 Pa, 60-100° C. to afford the title compound as a colourless oil (17.0 g, 59%).

후처리

  1. temperatureat reflux
  2. customfinally 11 g (37.8 mmol) 30 min
  3. additionAfter the addition
  4. temperaturethe mixture was heated
  5. temperatureat reflux for another 30 min
  6. temperatureThe reaction mixture was cooled
  7. distillationthe product was distilled at 25 Pa, 60-100° C.

출처 및 근거

ORD 기록
ord-7b92846416f54a358a6c43e185f2430a
출처 데이터셋
uspto-grants-2012_03
특허 번호
US08134007B2

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