8-Hydroxy-5-(1-hydroxy-2-((1-methylethyl)amino)butyl)-2(1H)-quinolinone → 5-(1-Hydroxy-2-isopropylaminobutyl)-8-p-methylbenzoyloxycarbostyril

HRID 27780

反応式

HRID 27780 の反応式
[OH:1][CH:2]([C:10]1[CH:19]=[CH:18][C:17]([OH:20])=[C:16]2[C:11]=1[CH:12]=[CH:13][C:14](=[O:21])[NH:15]2)[CH:3]([NH:6][CH:7]([CH3:9])[CH3:8])[CH2:4][CH3:5].[CH3:22][O-:23].[Na+]>CO>[OH:1][CH:2]([C:10]1[CH:19]=[CH:18][C:17]([O:20][C:22](=[O:23])[C:17]2[CH:18]=[CH:19][C:10]([CH3:2])=[CH:11][CH:16]=2)=[C:16]2[C:11]=1[CH:12]=[CH:13][C:14](=[O:21])[NH:15]2)[CH:3]([NH:6][CH:7]([CH3:9])[CH3:8])[CH2:4][CH3:5]

参加物

4

反応物 2

HCID 49168-Hydroxy-5-(1-hydroxy-2-((1-methylethyl)amino)butyl)-2(1H)-quinolinoneHCID 10942334Sodium Methoxide

生成物 1

HCID 233420685-(1-Hydroxy-2-isopropylaminobutyl)-8-p-methylbenzoyloxycarbostyril

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

5.8 g of 5-(1-hydroxy-2-isopropylaminobutyl)-8-hydroxycarbostyril was dissolved in 150 ml of methanol, and a 15% methanolic solution of sodium methylate was added to the solution in an equimolar amount relative to the starting carbostyryl compound. The mixture was concentrated to dryness and the resulting residue was dissolved in 100 ml of dimethylformamide. 3.0 g of p-toluylic acid chloride was added to the solution while cooling with ice-water, and the resulting mixture was stirred for 1.5 hours at room temperature. The precipitate formed was separated by filtration, and washed successively with dimethylformamide and diethyl ether to obtain 4.2 g of 5-(1-hydroxy-2-isopropylaminobutyl)-8-p-methylbenzoyloxycarbostyril having a melting point of 197°-198° C. (after recrystallization from chloroform-diethyl ether).

後処理

  1. concentrationThe mixture was concentrated to dryness
  2. dissolutionthe resulting residue was dissolved in 100 ml of dimethylformamide
  3. addition3.0 g of p-toluylic acid chloride was added to the solution
  4. temperaturewhile cooling with ice-water
  5. customThe precipitate formed
  6. customwas separated by filtration
  7. washwashed successively with dimethylformamide and diethyl ether

出典と根拠

ORDレコード
ord-6d5474d04144443dbbc59169da61ddb4
出典データセット
uspto-grants-1980_09
特許番号
US04223137

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