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Potassium Carbonate → HCID 14747672, 화합물

HRID 483850
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HRID 483850 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 1770652,6-DihydroxyquinolineHCID 20081659HCID 20081659, 화합물

생성물 1

HCID 14747672HCID 14747672, 화합물수율 10.3%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-aee4692f01f74a16acc0ccb0d8268667
출처 데이터셋
uspto-grants-1993_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05227381

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