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Water → HCID 20364450, 화합물

HRID 1678845
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HRID 1678845 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:9]23[CH2:18][CH2:17][CH2:16][CH:15]=[C:14]2[C:13](=[O:19])[NH:12][C:11](=[O:20])[CH2:10]3)[CH:6]=[CH:7][CH:8]=1.[H-].[Na+].S(O[CH2:28][CH2:29][C:30]1[CH:35]=[CH:34][C:33]([CH3:36])=[CH:32][CH:31]=1)(=O)(=O)C.O>CN(C)C=O>[CH3:36][C:33]1[CH:34]=[CH:35][C:30]([CH2:29][CH2:28][N:12]2[C:11](=[O:20])[CH2:10][C:9]3([C:5]4[CH:6]=[CH:7][CH:8]=[C:3]([O:2][CH3:1])[CH:4]=4)[C:14](=[CH:15][CH2:16][CH2:17][CH2:18]3)[C:13]2=[O:19])=[CH:31][CH:32]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 24758Sodium hydrideHCID 12942077HCID 12942077, 화합물HCID 132819714a-(m-Methoxyphenyl)-1,3-diketo-1,2,3,4,4a,5,6,7-octahydroisoquinoline

생성물 1

HCID 20364450HCID 20364450, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

4a-(m-Methoxyphenyl)-1,3-diketo-1,2,3,4,4a,5,6,7-octahydroisoquinoline (6 g) in 75 ml of anhydrous dimethylformamide was added to a 55% suspension of sodium hydride in mineral oil (1.2 g) in 50 ml of dimethylformamide at 70°. The reaction mixture was heated for one hour at 80° and then cooled to 25°. p-Methylphenethyl mesylate (7.0 g) was added and the reaction heated at 70° for 18 hours. It was poured into water and extracted with ether. The residue after evaporation of the ether was chromatographed on 800 g. of Florisil. This yielded 4.4 g, mp 134°-140°; recrystallized from ethanol, mp 149°-151°.

후처리

  1. temperatureThe reaction mixture was heated for one hour at 80°
  2. temperaturecooled to 25°
  3. temperaturethe reaction heated at 70° for 18 hours
  4. extractionextracted with ether
  5. customThe residue after evaporation of the ether
  6. customwas chromatographed on 800 g
  7. customrecrystallized from ethanol, mp 149°-151°

출처 및 근거

ORD 기록
ord-2dcaeb46f2c8445092c0000f26e8db7e
출처 데이터셋
uspto-grants-1978_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04077954

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