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

HRID 67076ノート

反応式

HRID 67076 の反応式
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][C:26]([Cl:29])=[CH:25][CH:24]=1)=[O:22].C(N(CC)CC)C>CO>[Cl:29][C:26]1[CH:27]=[CH:28][C:23]([C:21]([CH2:20][N:15]2[CH2:14][CH2:13][CH:12]([N:4]3[CH2:5][C:6]4[C:11](=[CH:10][CH:9]=[CH:8][CH:7]=4)[NH:2][C:3]3=[O:18])[CH2:17][CH2:16]2)=[O:22])=[CH:24][CH:25]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 68303p-Chlorophenacyl bromideHCID 183213553-(Piperidin-4-yl)-3,4-dihydroquinazolin-2(1H)-one hydrochloride

生成物 1

HCID 127979931-(4-Chlorobenzoylmethyl)-4-[3,4-dihydro-2(1H)-quinazolinon-3-yl]-piperidine収率 56%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

In this example, 4.0 g of 4-[3,4-dihydro-2(1H)-quinazolinon-3-yl]-piperidine mono-hydrochloride, 3.5 g of α-bromo-p-chloroacetophenone, 4.2 ml of triethylamine and 60 ml of methanol are mixed and stirred at room temperature overnight. The white crystals deposited are separated by filtration, successively washed with methanol and water and dried to obtain 5.17 g of a crude product. The crude product is recrystallized from a mixed solvent of chloroform and ethanol to obtain 3.21 g of the desired product.

後処理

  1. customThe white crystals deposited are separated by filtration
  2. washsuccessively washed with methanol and water
  3. customdried
  4. customto obtain 5.17 g of a crude product
  5. customThe crude product is recrystallized from a mixed solvent of chloroform and ethanol

出典と根拠

ORDレコード
ord-609aaef785044093b5b2a20a3ab02518
出典データセット
uspto-grants-1982_08
特許番号
US04344948

反応ノート

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