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Potassium Hydroxide → HCID 136027621, 화합물

HRID 1428845
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HRID 1428845 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]([CH:22]4[CH2:24][CH2:23]4)[CH:17]=3)[N:12]=2)[CH:10]=1)=[O:5])C.[OH-].[K+]>C1COCC1>[CH:22]1([C:16]2[CH:17]=[C:18]3[C:13](=[CH:14][CH:15]=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][C:19]3=[O:21])[CH2:23][CH2:24]1
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참가 물질

4

반응물 2

HCID 14797Potassium HydroxideHCID 136337170HCID 136337170, 화합물

생성물 1

HCID 136027621HCID 136027621, 화합물수율 85%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A mixture of 1-(6-cyclopropyl-4-oxo-3,4-dihydro-quinazolin-2-yl)-1H-pyrazole-4-carboxylic acid ethyl ester (0.045 g, 0.139 mmol), 1M aq. KOH (0.694 mL) and THF (0.694 mL) was stirred for 18 h. The mixture was concentrated to remove the THF and the aqueous residue was acidified with 6 M aq. HCl at 0° C. The resulting precipitate was collected by filtration to provide the titled compound (0.035 g, 85%). MS (ESI/Cl): mass calcd. for C16H12N4O3, 296.1; m/z found, 297.1 [M+H]+. 1H NMR (600 MHz, DMSO-d6): 12.92 (s, 2H), 8.93 (d, J=0.5 Hz, 1H), 8.24 (s, 1H), 7.81 (s, 1H), 7.65-7.50 (m, 2H), 2.22-2.04 (m, 1H), 1.14-0.94 (m, 2H), 0.85-0.68 (m, 2H).

후처리

  1. concentrationThe mixture was concentrated
  2. customto remove the THF
  3. customwas acidified with 6 M aq. HCl at 0° C
  4. filtrationThe resulting precipitate was collected by filtration

출처 및 근거

ORD 기록
ord-aa11025f13c04891a8b83e792c30cad8
출처 데이터셋
uspto-grants-2015_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08937078B2

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