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Potassium Carbonate → HCID 14747672、化合物

HRID 483850
ノート
印刷プレビュー

反応式

HRID 483850 の反応式
[OH:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[NH:8][C:7](=[O:12])[CH:6]=[CH:5]2.C([O-])([O-])=O.[K+].[K+].[N:19]1([CH2:24][CH2:25][N:26]([CH2:34][CH:35]2[CH2:40][CH2:39][CH2:38][CH2:37][CH2:36]2)[C:27](=[O:33])[CH2:28][CH2:29][CH2:30][CH2:31]Cl)[CH2:23][CH2:22][CH2:21][CH2:20]1>CN(C)C=O>[N:19]1([CH2:24][CH2:25][N:26]([CH2:34][CH:35]2[CH2:40][CH2:39][CH2:38][CH2:37][CH2:36]2)[C:27]([CH2:28][CH2:29][CH2:30][CH2:31][O:1][C:2]2[CH:3]=[C:4]3[C:9](=[CH:10][CH:11]=2)[NH:8][C:7](=[O:12])[CH:6]=[CH:5]3)=[O:33])[CH2:23][CH2:22][CH2:21][CH2:20]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 1770652,6-DihydroxyquinolineHCID 20081659HCID 20081659、化合物

生成物 1

HCID 14747672HCID 14747672、化合物収率 10.3%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To 50 ml of dimethylformamide are added 1.73 g of 6-hydroxycarbostyril, 1.8 g of K2CO3 and 0.5 g of KI. To this mixture being stirred at 60°-70° C. is dropwise added 4.2 g of N-[2-(1-pyrrolidinyl)ethyl]-N-(5-chloropentanoyl)-cyclohexylmethylamine. Then, the mixture is stirred for 4 hours at the same temperature. The solvent is removed by evaporation. The residue is dissolved in 200 ml of chloroform and the solution is washed with diluted hydrochloric acid, a 1% aqueous sodium hydroxide solution and water in this order, and dried with anhydrous magnesium sulfate. The desiccant is removed by filtration and the filtrate is concentrated. The residue is purified by means of a silica gel column chromatography (eluent; chloroform:methanol=20:1) and recrystallized from diethyl ether to obtain 0.5 g of 6-[4-{N-[2-(1-pyrrolidinyl)ethyl]-N-cyclohexylmethylaminocarbonyl}-butoxy]carbostyril.

後処理

  1. stirringThen, the mixture is stirred for 4 hours at the same temperature
  2. customThe solvent is removed by evaporation
  3. dissolutionThe residue is dissolved in 200 ml of chloroform
  4. washthe solution is washed with diluted hydrochloric acid
  5. dry with materiala 1% aqueous sodium hydroxide solution and water in this order, and dried with anhydrous magnesium sulfate
  6. customThe desiccant is removed by filtration
  7. concentrationthe filtrate is concentrated
  8. customThe residue is purified by means of a silica gel column chromatography (eluent; chloroform:methanol=20:1)
  9. customrecrystallized from diethyl ether

出典と根拠

ORDレコード
ord-aee4692f01f74a16acc0ccb0d8268667
出典データセット
uspto-grants-1993_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05227381

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート