Water → HCID 23471608, 화합물

HRID 128015노트

반응식

HRID 128015 반응식
[CH3:1][CH:2]1[C:7]([C:8]2[CH:9]=[C:10]3[C:15](=[CH:16][CH:17]=2)[N:14]([CH3:18])[C:13](=[O:19])[CH2:12][CH2:11]3)=[N:6][NH:5][C:4](=[O:20])[CH2:3]1.[H-].[Na+].[CH2:23](Br)[CH3:24].O>CN(C)C=O>[CH2:23]([N:5]1[C:4](=[O:20])[CH2:3][CH:2]([CH3:1])[C:7]([C:8]2[CH:9]=[C:10]3[C:15](=[CH:16][CH:17]=2)[N:14]([CH3:18])[C:13](=[O:19])[CH2:12][CH2:11]3)=[N:6]1)[CH3:24]

참가 물질

6

반응물 4

HCID 962WaterHCID 6332Ethyl BromideHCID 24758Sodium hydrideHCID 129826Y 590

생성물 1

HCID 23471608HCID 23471608, 화합물수율 62.1%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of 5.4 g of 6-(5-methyl-3-oxo-2,3,4,5-tetrahydropyridazin-6-yl)-1-methyl-1,2,3,4-tetrahydroquinolin-2-one in 50 ml of dimethylformamide was added 1.1 g of 50% sodium hydride. After stirring for about 30 minutes, 2.4 g of ethyl bromide was added and the mixture was stirred at about 40° C. for one hour. The reaction mixture was poured into 200 ml of water and extracted with 100 ml of ethyl acetate. The extract was dried over magnesium sulfate and concentrated under reduced pressure. The residue was recrystallized from ethanol to give 3.7 g of 6-(2-ethyl-5-methyl-3-oxo-2,3,4,5-tetrahydropyridazin-6-yl)-1-methyl-1,2,3,4-tetrahydroquinolin-2-one as colorless crystals, melting at 170°-172° C.

후처리

  1. stirringthe mixture was stirred at about 40° C. for one hour
  2. extractionextracted with 100 ml of ethyl acetate
  3. dry with materialThe extract was dried over magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe residue was recrystallized from ethanol

출처 및 근거

ORD 기록
ord-d2608a36971a4ce193abc04e18bcc191
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04258185

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