Potassium Phosphate, Tribasic → (S)-N2-[1-(4-Fluorophenyl)ethyl]-N4-(pyrazin-2-yl)-6-(thiazol-5-yl)pyrimidine-2,4-diamine
반응식
Cl[C:2]1[CH:7]=[C:6]([C:8]2[S:12][CH:11]=[N:10][CH:9]=2)[N:5]=[C:4]([NH:13][C@H:14]([C:16]2[CH:21]=[CH:20][C:19]([F:22])=[CH:18][CH:17]=2)[CH3:15])[N:3]=1.[NH2:23][C:24]1[CH:29]=[N:28][CH:27]=[CH:26][N:25]=1.P([O-])([O-])([O-])=O.[K+].[K+].[K+]>O1CCOCC1>[F:22][C:19]1[CH:20]=[CH:21][C:16]([C@@H:14]([NH:13][C:4]2[N:3]=[C:2]([NH:23][C:24]3[CH:29]=[N:28][CH:27]=[CH:26][N:25]=3)[CH:7]=[C:6]([C:8]3[S:12][CH:11]=[N:10][CH:9]=3)[N:5]=2)[CH3:15])=[CH:17][CH:18]=1참가 물질
반응물 3
생성물 1
시약·촉매·용매 1
반응 조건
- 온도
- 100 °C
실험 절차
To 155 mg of (S)-4-chloro-N-[1-(4-fluorophenyl)ethyl]-6-(thiazol-5-yl)pyrimidine-2-amine, 53 mg of 2-aminopyrazine, 72 mg of 4,5-bis(diphenylphosphino)-9,9′-dimethylxanthene, 196 mg of tripotassium phosphate and 81 mg of tris(dibenzylideneacetone)(chloroform)dipalladium, was added 4 ml of 1,4-dioxane, and the mixture was subjected to degassing, and substituted by argon gas, and then was stirred at 100° C. for 5 hours. The reaction solution was diluted with ethyl acetate. The solution was washed in turn with water and brine and then dried over magnesium sulfate. The solvent was distilled off under reduced pressure, and then the obtained residue was purified by silica gel column chromatography to obtain 105 mg of the objective compound as pale yellow powder.
후처리
- customto degassing
- additionThe reaction solution was diluted with ethyl acetate
- washThe solution was washed in turn with water and brine
- dry with materialdried over magnesium sulfate
- distillationThe solvent was distilled off under reduced pressure
- customthe obtained residue was purified by silica gel column chromatography
출처 및 근거
- ORD 기록
- ord-a2a46c609f6144308d5fad6d82acefed
- 출처 데이터셋
- uspto-grants-2014_03
- 특허 번호
- US08673891B2
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