Hydrochloric Acid → HCID 136337191、化合物

HRID 1428886ノート

反応式

HRID 1428886 の反応式
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]

参加物

4

反応物 3

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 68488561HCID 68488561、化合物

生成物 1

HCID 136337191HCID 136337191、化合物収率 53%

反応条件

温度
23 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-9fa7edfafff04ce984fe4813347fe65a
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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