Trifluoroacetic acid → 1-(4-Fluoro-phenyl)-2-oxo-1,2-dihydro-pyridine-3-carboxylic acid[1-methyl-6-(2-oxo-1,2,3,4-tetrahydro-pyrido[2,3-d]pyrimidin-5-yloxy)-1H-indazol-3-yl]-amide

HRID 1045507

반응식

HRID 1045507 반응식
COC1C=CC(C[N:8]2[CH2:13][C:12]3[C:14]([O:18][C:19]4[CH:27]=[C:26]5[C:22]([C:23]([NH:29][C:30]([C:32]6[C:33](=[O:45])[N:34]([C:38]7[CH:43]=[CH:42][C:41]([F:44])=[CH:40][CH:39]=7)[CH:35]=[CH:36][CH:37]=6)=[O:31])=[N:24][N:25]5[CH3:28])=[CH:21][CH:20]=4)=[CH:15][CH:16]=[N:17][C:11]=3[NH:10][C:9]2=[O:46])=CC=1.FC(F)(F)C(O)=O>>[CH3:28][N:25]1[C:26]2[C:22](=[CH:21][CH:20]=[C:19]([O:18][C:14]3[C:12]4[CH2:13][NH:8][C:9](=[O:46])[NH:10][C:11]=4[N:17]=[CH:16][CH:15]=3)[CH:27]=2)[C:23]([NH:29][C:30]([C:32]2[C:33](=[O:45])[N:34]([C:38]3[CH:39]=[CH:40][C:41]([F:44])=[CH:42][CH:43]=3)[CH:35]=[CH:36][CH:37]=2)=[O:31])=[N:24]1

참가 물질

3

반응물 2

HCID 6422Trifluoroacetic acidHCID 704970111-(4-Fluoro-phenyl)-2-oxo-1,2-dihydro-pyridine-3-carboxylicacid{6-[3-(4-methoxy-benzyl)-2-oxo-1,2,3,4-tetrahydro-pyrido[2,3-d]pyrimidin-5-yloxy]-1-methyl-1H-indazol-3-yl}-amide

생성물 1

HCID 704982091-(4-Fluoro-phenyl)-2-oxo-1,2-dihydro-pyridine-3-carboxylic acid[1-methyl-6-(2-oxo-1,2,3,4-tetrahydro-pyrido[2,3-d]pyrimidin-5-yloxy)-1H-indazol-3-yl]-amide수율 82.5%

반응 조건

온도
80 °C

실험 절차

A solution of compound 278 (22.00 mg; 0.03 mmol; 1.00 eq.) and trifluoroacetic acid (2.00 ml) was stirred at 80 degrees C. overnight. The reaction was stirred at 80 degrees C. for 22 hr. The reaction was concentrated, redissolved in DMSO, and treated with Et3N to pH 8. The solution was then purified directly via prep HPLC to afford 13 mg (60%) of 279 as a yellow solid. LC-MS (M+H=526, obsd.=526).

후처리

  1. customovernight
  2. concentrationThe reaction was concentrated
  3. dissolutionredissolved in DMSO
  4. additiontreated with Et3N to pH 8
  5. customThe solution was then purified directly via prep HPLC

출처 및 근거

ORD 기록
ord-e29d7cace7f14278a10abbbf4ee75ec7
출처 데이터셋
uspto-grants-2013_10
특허 번호
US08569295B2

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