Hydrochloric Acid → HCID 136337191, 화합물

HRID 1428886노트

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HRID 1428886 반응식
Cl.O1CCOCC1.[CH2:8]([O:10][C:11]([C:13]1[CH:14]=[N:15][N:16]([C:18]2[N:27](COCCOC)[C:26](=[O:34])[C:25]3[C:20](=[CH:21][C:22]([C:35]4[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=4)=[CH:23][CH:24]=3)[N:19]=2)[CH:17]=1)=[O:12])[CH3:9]>>[CH2:8]([O:10][C:11]([C:13]1[CH:14]=[N:15][N:16]([C:18]2[NH:27][C:26](=[O:34])[C:25]3[C:20](=[CH:21][C:22]([C:35]4[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=4)=[CH:23][CH:24]=3)[N:19]=2)[CH:17]=1)=[O:12])[CH3:9]

참가 물질

4

반응물 3

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 68488561HCID 68488561, 화합물

생성물 1

HCID 136337191HCID 136337191, 화합물수율 53%

반응 조건

온도
23 °C

실험 절차

A solution of 4M HCl and dioxane (3.00 mL, 12.0 mmol) was added to 1-[3-(2-methoxy-ethoxymethyl)-4-oxo-7-phenyl-3,4-dihydro-quinazolin-2-yl]-1H-pyrazole-4-carboxylic acid ethyl ester (90.0 mg, 0.201 mmol). The reaction mixture was stirred at 23° C. After 18 h, the reaction mixture was concentrated under reduced pressure. Et2O was added (5 mL) and the resulting precipitate was collected by filtration and washed well with Et2O to afford the titled compound (38.0 mg, 53%). MS (ESI): mass calcd. for C20H16N4O3, 360.1; m/z found, 361.1 [M+H]+. 1H NMR (600 MHz, DMSO-d6): 12.93 (s, 1H), 9.04 (s, 1H), 8.34 (s, 1H), 8.20 (d, J=8.2 Hz, 1H), 7.98 (s, 1H), 7.84 (dd, J=10.5, 4.2 Hz, 3H), 7.55 (t, J=7.6 Hz, 2H), 7.49-7.46 (m, 1H), 4.31 (q, J=7.1 Hz, 2H), 1.33 (t, J=7.1 Hz, 3H).

후처리

  1. concentrationthe reaction mixture was concentrated under reduced pressure
  2. additionEt2O was added (5 mL)
  3. filtrationthe resulting precipitate was collected by filtration
  4. washwashed well with Et2O

출처 및 근거

ORD 기록
ord-9fa7edfafff04ce984fe4813347fe65a
출처 데이터셋
uspto-grants-2015_01
특허 번호
US08937078B2

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