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Chloroform → 5-[4-(4-Methylbenzoyl)-1-piperazinyl]-3,4-dihydrocarbostyril

HRID 1649220
ノート
印刷プレビュー

反応式

HRID 1649220 の反応式
[N:1]1([C:7]2[CH:16]=[CH:15][CH:14]=[C:13]3[C:8]=2[CH2:9][CH2:10][C:11](=[O:17])[NH:12]3)[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.C(N(CC)CC)C.C(Cl)(Cl)Cl.[CH3:29][C:30]1[CH:38]=[CH:37][C:33]([C:34](Cl)=[O:35])=[CH:32][CH:31]=1>O>[CH3:29][C:30]1[CH:38]=[CH:37][C:33]([C:34]([N:4]2[CH2:5][CH2:6][N:1]([C:7]3[CH:16]=[CH:15][CH:14]=[C:13]4[C:8]=3[CH2:9][CH2:10][C:11](=[O:17])[NH:12]4)[CH2:2][CH2:3]2)=[O:35])=[CH:32][CH:31]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6212Chloroform3 回HCID 8471TriethylamineHCID 134054-Methylbenzoyl ChlorideHCID 11630008HCID 11630008、化合物

生成物 1

HCID 132363395-[4-(4-Methylbenzoyl)-1-piperazinyl]-3,4-dihydrocarbostyril収率 45.8%

試薬・触媒・溶媒 1

HCID 962Water
溶媒

実験手順

5-(1-Piperazinyl)-3,4-dihydrocarbostyril (2.6 g) and 2.34 ml of triethylamine were added to 50 ml of chloroform. The mixture was stirred at room temperature while slowly adding dropwise 10 ml of chloroform solution containing 2.3 g of 4-methylbenzoyl chloride. After completion of addition, the reaction mixture was stirred for 30 minutes. After completion of reaction, 100 ml of chloroform and then a large amount of water was added to separate chloroform and the chloroform layer was washed with sodium hydrogencarbonate solution and subsequently with water and dried over anhydrous sodium sulfate. Chloroform was distilled off and residual crystals were recrystallized from chloroformether to give 1.8 g of 5-[4-(4-methylbenzoyl)-1-piperazinyl]-3,4-dihydrocarbostyril, m.p. 239.5°-240° C., colorless powders.

後処理

  1. additionAfter completion of addition
  2. stirringthe reaction mixture was stirred for 30 minutes
  3. customto separate chloroform
  4. washthe chloroform layer was washed with sodium hydrogencarbonate solution and subsequently with water
  5. dry with materialdried over anhydrous sodium sulfate
  6. distillationChloroform was distilled off
  7. customresidual crystals were recrystallized from chloroformether

出典と根拠

ORDレコード
ord-df8d394e4a35424e9270e2f5321cfc4f
出典データセット
uspto-grants-1983_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04415572

反応ノート

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