8-Hydroxy-5-(1-hydroxy-2-((1-methylethyl)amino)butyl)-2(1H)-quinolinone → HCID 23342075, 화합물

HRID 27779

반응식

HRID 27779 반응식
[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].C[O-:23].[Na+].N1[C:35]2[C:30](=[CH:31][CH:32]=[CH:33][CH:34]=2)[CH:29]=CC1=O>CO>[CH:30]1([C:29]([O:20][C:17]2[CH:18]=[CH:19][C:10]([CH:2]([OH:1])[CH:3]([NH:6][CH:7]([CH3:9])[CH3:8])[CH2:4][CH3:5])=[C:11]3[C:16]=2[NH:15][C:14](=[O:21])[CH:13]=[CH:12]3)=[O:23])[CH2:35][CH2:34][CH2:33][CH2:32][CH2:31]1

참가 물질

5

반응물 3

HCID 49168-Hydroxy-5-(1-hydroxy-2-((1-methylethyl)amino)butyl)-2(1H)-quinolinoneHCID 60382-HydroxyquinolineHCID 10942334Sodium Methoxide

생성물 1

HCID 23342075HCID 23342075, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
0 °C

실험 절차

5.8 g of 5-(1-hydroxy-2-isopropylaminobutyl)-8-hydroxycarbostyril was dissolved in 100 ml of methanol, and a methanolic solution of 10% sodium methylate was added to the resulting solution in an equimolar amount relative to the starting carbostyril compound. The mixture was concentrated to dryness and the resulting residue was dissolved in 100 ml of dimethylformamide. 2.9 g of cyclohexanecarboxylic acid chloride was then added while cooling with ice-water and the mixture was stirred for one hour at a temperature of 0° C. The precipitate formed was separated by filtration and washed successively with dimethylformamide and diethyl ether to obtain 4.0 g of 8-cyclohexylcarbonyloxy-5-(1-hydroxy-2-isopropylaminobutyl)carbostyril having a melting point of 186.5°-187.5° C. (after recrystallization from chloroform-diethyl ether).

후처리

  1. concentrationThe mixture was concentrated to dryness
  2. dissolutionthe resulting residue was dissolved in 100 ml of dimethylformamide
  3. addition2.9 g of cyclohexanecarboxylic acid chloride was then added
  4. temperaturewhile cooling with ice-water
  5. customThe precipitate formed
  6. customwas separated by filtration
  7. washwashed successively with dimethylformamide and diethyl ether

출처 및 근거

ORD 기록
ord-f3590321f0f643f4a964e0c3575330c3
출처 데이터셋
uspto-grants-1980_09
특허 번호
US04223137

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