2-Hydroxyquinoline → HCID 23342064、化合物

HRID 27782

反応式

HRID 27782 の反応式
Cl.[OH:2][CH:3]([C:11]1[CH:20]=[CH:19][C:18]([OH:21])=[C:17]2[C:12]=1[CH2:13][CH2:14][C:15](=[O:22])[NH:16]2)[CH:4]([NH:7][CH:8]([CH3:10])[CH3:9])[CH2:5][CH3:6].[CH3:23][O-:24].[Na+].N1[C:36]2[C:31](=[CH:32][CH:33]=[CH:34][CH:35]=2)[CH:30]=CC1=O>CO>[OH:2][CH:3]([C:11]1[CH:20]=[CH:19][C:18]([O:21][C:23](=[O:24])[C:34]2[CH:33]=[CH:32][C:31]([CH3:30])=[CH:36][CH:35]=2)=[C:17]2[C:12]=1[CH2:13][CH2:14][C:15](=[O:22])[NH:16]2)[CH:4]([NH:7][CH:8]([CH3:10])[CH3:9])[CH2:5][CH3:6]

参加物

5

反応物 3

HCID 60382-HydroxyquinolineHCID 10942334Sodium MethoxideHCID 233421115-(1-Hydroxy-2-isopropylaminobutyl)-8-hydroxy-3,4-dihydrocarbostyril hydrochloride

生成物 1

HCID 23342064HCID 23342064、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

3.28 g of 5-(1-hydroxy-2-isopropylaminobutyl)-8-hydroxy-3,4-dihydrocarbostyril hydrochloride was dissolved in 50 ml of methanol, and a 20% methanolic solution of sodium methylate was added to the solution in an amount of 2 moles per mole of the starting carbostyril compound. The mixture was then concentrated to dryness, and the residue was dissolved in dimethylformamide. 1.7 g of p-toluylic acid chloride was added to the solution while cooling with ice-water and the mixture was stirred for 4 hours at room temperature. The reaction mixture was poured into ice-water and extracted with chloroform. A mixture of diethyl ether and petroleum benzene was added to the chloroform extract to obtain 1.94 g of crystalline 5-(1-hydroxy-2-isopropylaminobutyl)-8-p-methylbenzoyloxy-3,4-dihydrocarbostyril having a melting point of 151.5°-152.5° C. (after recrystallization from chloroform-n-hexane).

後処理

  1. concentrationThe mixture was then concentrated to dryness
  2. dissolutionthe residue was dissolved in dimethylformamide
  3. addition1.7 g of p-toluylic acid chloride was added to the solution
  4. temperaturewhile cooling with ice-water
  5. additionThe reaction mixture was poured into ice-water
  6. extractionextracted with chloroform
  7. additionA mixture of diethyl ether and petroleum benzene
  8. additionwas added to the chloroform
  9. extractionextract

出典と根拠

ORDレコード
ord-e1037e8dd75547f1aadf9b0d660bb31b
出典データセット
uspto-grants-1980_09
特許番号
US04223137

関連ノート

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