Trifluoroacetic acid → HCID 22030922、化合物

HRID 454189ノート

反応式

HRID 454189 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[O:13][CH2:14][CH2:15][CH2:16][N:17]1[CH2:22][CH2:21][O:20][CH2:19][CH2:18]1)[N:9]=[CH:8][N:7]=[C:6]2[O:23][C:24]1[CH:25]=[C:26]2[C:31](=[CH:32][CH:33]=1)[N:30](C(OC(C)(C)C)=O)[CH2:29][CH2:28][CH2:27]2.C(O)(C(F)(F)F)=O>ClCCl>[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[O:13][CH2:14][CH2:15][CH2:16][N:17]1[CH2:22][CH2:21][O:20][CH2:19][CH2:18]1)[N:9]=[CH:8][N:7]=[C:6]2[O:23][C:24]1[CH:25]=[C:26]2[C:31](=[CH:32][CH:33]=1)[NH:30][CH2:29][CH2:28][CH2:27]2

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 22030734HCID 22030734、化合物

生成物 1

HCID 22030922HCID 22030922、化合物収率 93.2%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To 6-methoxy-7-(3-morpholinopropoxy)-4-((1-tertbutoxycarbonyl-1,2,3,4-tetrahydroquinolin-6-yl)oxy)quinazoline (110 mg, 0.2 mmol) in solution in dichloromethane (3 ml) was added TFA (0.3 ml) and the mixture stirred for 1 hour at ambient temperature. The solvents were evaporated and the remaining oil was diluted with dichloromethane and the pH adjusted to 9 with a saturated solution of sodium hydrogen carbonate. The organic phase was washed with, brine, dried (MgSO4), filtered and the solvent evaporated to give 6-methoxy-7-(3-morpholinopropoxy)-4-(1,2,3,4-tetrahydroquinolin-6-yloxy)quinazoline (84 mg, 93%).

後処理

  1. customThe solvents were evaporated
  2. additionthe remaining oil was diluted with dichloromethane
  3. washThe organic phase was washed with, brine
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. customthe solvent evaporated

出典と根拠

ORDレコード
ord-5733ebc89b2c48c98e6102c2636229c1
出典データセット
uspto-grants-2013_07
特許番号
US08492560B2

反応ノート

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