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

反応式

HRID 1045507 の反応式
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

参加物

3

反応物 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

生成物 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]-amide収率 82.5%

反応条件

温度
80 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-e29d7cace7f14278a10abbbf4ee75ec7
出典データセット
uspto-grants-2013_10
特許番号
US08569295B2

関連ノート

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