Triethylamine → 1-(3-chlorobenzoylmethyl)-4-[3,4-dihydro-2(1H)-quinazolinon-3-yl]-piperidine

HRID 67075

반응식

HRID 67075 반응식
Cl.[NH:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[CH2:5][N:4]([CH:12]2[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]2)[C:3]1=[O:18].Br[CH2:20][C:21]([C:23]1[CH:28]=[CH:27][CH:26]=[C:25]([Cl:29])[CH:24]=1)=[O:22].C(N(CC)CC)C>CO>[Cl:29][C:25]1[CH:24]=[C:23]([CH:28]=[CH:27][CH:26]=1)[C:21]([CH2:20][N:15]1[CH2:14][CH2:13][CH:12]([N:4]2[CH2:5][C:6]3[C:11](=[CH:10][CH:9]=[CH:8][CH:7]=3)[NH:2][C:3]2=[O:18])[CH2:17][CH2:16]1)=[O:22]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 387382-Bromo-3'-chloroacetophenoneHCID 183213553-(Piperidin-4-yl)-3,4-dihydroquinazolin-2(1H)-one hydrochloride

생성물 1

HCID 127979921-(3-chlorobenzoylmethyl)-4-[3,4-dihydro-2(1H)-quinazolinon-3-yl]-piperidine수율 50.4%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

In this example, 2.67 g of 4-[3,4-dihydro-2(1H)-quinazolinon-3-yl]-piperidine mono-hydrochloride, 2.33 g of α-bromo-m-chloroacetophenone, 2.8 ml of triethylamine and 30 ml of methanol are mixed and stirred at room temperature overnight. Then, the white crystals deposited are separated by filtration, successively washed with methanol and water and dried to obtain 2.89 g of a crude product. The crude product is recrystallized from a mixed solvent of chloroform and ethanol to obtain 1.93 g of the desired product.

후처리

  1. customThen, the white crystals deposited are separated by filtration
  2. washsuccessively washed with methanol and water
  3. customdried
  4. customto obtain 2.89 g of a crude product
  5. customThe crude product is recrystallized from a mixed solvent of chloroform and ethanol

출처 및 근거

ORD 기록
ord-1f54b4acf24a4bcbaa663e740ddf1acb
출처 데이터셋
uspto-grants-1982_08
특허 번호
US04344948

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