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Water → HCID 86621097, 화합물

HRID 1620864
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인쇄 미리보기

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HRID 1620864 반응식
C([O-])([O-])=O.[Cs+].[Cs+].[F:7][C:8]([F:24])([F:23])[CH:9]([C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=1[C:17]1[CH:18]=[N:19][CH:20]=[N:21][CH:22]=1)[OH:10].[NH2:25][C:26]1[N:31]=[C:30](Cl)[CH:29]=[C:28]([Cl:33])[N:27]=1.O>C1COCC1.C(OCC)(=O)C>[Cl:33][C:28]1[CH:29]=[C:30]([O:10][CH:9]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2[C:17]2[CH:22]=[N:21][CH:20]=[N:19][CH:18]=2)[C:8]([F:7])([F:23])[F:24])[N:31]=[C:26]([NH2:25])[N:27]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

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HCID 962WaterHCID 10796Cesium carbonateHCID 655222-Amino-4,6-dichloropyrimidineHCID 667435372-(5-Pyrimidinyl)-α-(trifluoromethyl)benzenemethanol

생성물 1

HCID 86621097HCID 86621097, 화합물수율 92%

시약·촉매·용매 2

HCID 8028Tetrahydrofuran
용매
HCID 8857Ethyl Acetate용매

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온도
110 °C

실험 절차

Cs2CO3 (325 mg, 1.0 mmol) was added to a solution of 2,2,2-trifluoro-1-(2-pyrimidin-5-yl-phenyl)-ethanol (72 mg, 0.28 mmol) in 10 ml of anhydrous THF. The mixture was stirred for 20 min, 2-amino-4,6-dichloro-pyrimidine (36.7 mg, 0.22 mmol) was added and then the reaction mixture was heated at 110° C. until the reaction was completed. After cooling to room temperature, 5 ml of water was added and ethyl acetate (20 ml) was used to extract the product. The organic layer was dried over sodium sulfate. The solvent was removed by rotovap to give 76 mg of crude 4-chloro-6-[2,2,2-trifluoro-1-(2-pyrimidin-5-yl-phenyl)-ethoxy]-pyrimidin-2-ylamine (yield: 92%).

후처리

  1. temperatureAfter cooling to room temperature
  2. extractionto extract the product
  3. dry with materialThe organic layer was dried over sodium sulfate
  4. customThe solvent was removed by rotovap

출처 및 근거

ORD 기록
ord-679e4f95179447c3ada58e274713c7b0
출처 데이터셋
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08772482B2

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