Hydrochloric Acid → HCID 136337162, 화합물

HRID 1428829노트

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HRID 1428829 반응식
Cl.O1CCOCC1.[CH2:8]([O:10][C:11]([C:13]1[CH:14]=[N:15][N:16]([C:18]2[N:27](COCC[Si](C)(C)C)[C:26](=[O:36])[C:25]3[C:20](=[CH:21][CH:22]=[C:23]([C:37]4[CH:42]=[CH:41][CH:40]=[CH:39][C:38]=4[CH3:43])[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:36])[C:25]3[C:20](=[CH:21][CH:22]=[C:23]([C:37]4[CH:42]=[CH:41][CH:40]=[CH:39][C:38]=4[CH3:43])[CH:24]=3)[N:19]=2)[CH:17]=1)=[O:12])[CH3:9]

참가 물질

4

반응물 3

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 68487879HCID 68487879, 화합물

생성물 1

HCID 136337162HCID 136337162, 화합물수율 80%

반응 조건

온도
23 °C

실험 절차

A solution of HCl in dioxane (4M, 0.872 mL, 3.48 mmol) was added to 1-[4-oxo-6-o-tolyl-3-(2-trimethylsilanyl-ethoxymethyl)-3,4-dihydro-quinazolin-2-yl]-1H-pyrazole-4-carboxylic acid ethyl ester (88.0 mg, 0.174 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 (52.0 mg, 80%). MS (ESI): mass calcd. for C21H18N4O3, 374.1; m/z found 375.2 [M+H]+. 1H NMR (600 MHz, CDCl3): 9.05 (s, 1H), 8.35 (s, 1H), 8.02 (s, 1H), 7.86 (d, J=6.6 Hz, 1H), 7.78 (s, 1H), 7.37-7.28 (m, 4H), 4.31 (q, J=7.1 Hz, 2H), 2.28 (s, 3H), 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-8af44849201245d284057e3a83666583
출처 데이터셋
uspto-grants-2015_01
특허 번호
US08937078B2

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