Hydrochloric Acid → HCID 59556306, 화합물

HRID 1172664노트

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HRID 1172664 반응식
[CH3:1][C:2]1[N:3]=[C:4]([C:9]2[CH:14]=[CH:13][C:12]([C:15]([F:18])([F:17])[F:16])=[CH:11][CH:10]=2)[S:5][C:6]=1[CH:7]=[O:8].Br[C:20]([F:24])([F:23])[CH:21]=[CH2:22].Cl>CN(C)C=O>[F:23][C:20]([F:24])([CH:21]=[CH2:22])[CH:7]([C:6]1[S:5][C:4]([C:9]2[CH:10]=[CH:11][C:12]([C:15]([F:18])([F:16])[F:17])=[CH:13][CH:14]=2)=[N:3][C:2]=1[CH3:1])[OH:8]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 5550853-bromo-3,3-difluoroprop-1-eneHCID 27828994-Methyl-2-[4-(trifluoromethyl)phenyl]-1,3-thiazole-5-carbaldehyde

생성물 1

HCID 59556306HCID 59556306, 화합물수율 57.5%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of 1.0 g 4-Methyl-2-(4-trifluoromethyl-phenyl)-thiazole-5-carbaldehyde and 868 mg 3-bromo-3,3-difluorpropene in 10 ml dimethylformamide 425 mg Indium were added and the resulting suspension was stirred in an ultrasonic bath for two hours. Then 20 ml 1 N hydrochloric acid were added and the mixture stirred at room temperature for thirty minutes. The mixture was extracted three times with portions of 50 ml ethyl acetate. The combined organic layers were dried over MgSO4. The solvent was evaporated in vacuo. The resulting residue was purified by reversed phase HPLC to obtain 740 mg 2,2-Difluoro-1-[4-methyl-2-(4-trifluoromethyl-phenyl)-thiazol-5-yl]-but-3-en-1-ol as a colorless lyophilisate.

후처리

  1. stirringthe mixture stirred at room temperature for thirty minutes
  2. extractionThe mixture was extracted three times with portions of 50 ml ethyl acetate
  3. dry with materialThe combined organic layers were dried over MgSO4
  4. customThe solvent was evaporated in vacuo
  5. customThe resulting residue was purified by reversed phase HPLC

출처 및 근거

ORD 기록
ord-51237ab247af471281c0608f9fa68260
출처 데이터셋
uspto-grants-2010_11
특허 번호
US07834030B2

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