Potassium Hydroxide → HCID 135895253、化合物

HRID 1428830ノート

反応式

HRID 1428830 の反応式
C([O:3][C:4]([C:6]1[CH:7]=[N:8][N:9]([C:11]2[NH:20][C:19](=[O:21])[C:18]3[C:13](=[CH:14][CH:15]=[C:16]([C:22]4[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=4[CH3:28])[CH:17]=3)[N:12]=2)[CH:10]=1)=[O:5])C.[OH-].[K+]>C1COCC1>[O:21]=[C:19]1[C:18]2[C:13](=[CH:14][CH:15]=[C:16]([C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=3[CH3:28])[CH:17]=2)[N:12]=[C:11]([N:9]2[CH:10]=[C:6]([C:4]([OH:5])=[O:3])[CH:7]=[N:8]2)[NH:20]1

参加物

4

反応物 2

HCID 14797Potassium HydroxideHCID 136337162HCID 136337162、化合物

生成物 1

HCID 135895253HCID 135895253、化合物収率 81%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A mixture of 1-(4-oxo-6-o-tolyl-3,4-dihydro-quinazolin-2-yl)-1H-pyrazole-4-carboxylic acid ethyl ester (40.0 mg, 1.07 mmol), 1M aq. KOH (0.5 mL) and THF (1 mL) was stirred for 16 h. The reaction mixture was concentrated under reduced pressure to remove the THF and the aqueous residue was acidified to pH 2 with 1 M aq. HCl. The resulting precipitate was collected by filtration to provide the titled compound (30.0 mg, 81%). MS (ESI): mass calcd. for C19H14N4O3, 346.1; m/z found 347.0 [M+H]+. 1H NMR (600 MHz, DMSO-d6): 13.04 (s, 1H), 12.93 (s, 1H), 8.99 (s, 1H), 8.28 (s, 1H), 8.02 (s, 1H), 7.86 (d, J=7.5 Hz, 1H), 7.76 (d, J=7.8 Hz, 1H), 7.37-7.29 (m, 4H), 2.28 (s, 3H).

後処理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. customto remove the THF
  3. filtrationThe resulting precipitate was collected by filtration

出典と根拠

ORDレコード
ord-3b64d7d1127d4dc984cdde1c51e67dd6
出典データセット
uspto-grants-2015_01
特許番号
US08937078B2

反応ノート

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