Potassium Hydroxide → HCID 135895253, 화합물

HRID 1428830노트

반응식

HRID 1428830 반응식
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

참가 물질

4

반응물 2

HCID 14797Potassium HydroxideHCID 136337162HCID 136337162, 화합물

생성물 1

HCID 135895253HCID 135895253, 화합물수율 81%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-3b64d7d1127d4dc984cdde1c51e67dd6
출처 데이터셋
uspto-grants-2015_01
특허 번호
US08937078B2

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