Triethylamine → 4-Acetyl-8-chloro-1,1-dimethyl-1,2,3,4,5,6-hexahydrobenzo[f]quinoline

HRID 2051344노트

반응식

HRID 2051344 반응식
[Cl:1][C:2]1[CH:17]=[CH:16][C:5]2[C:6]3[C:7]([CH3:15])([CH3:14])[CH2:8][CH2:9][NH:10][C:11]=3[CH2:12][CH2:13][C:4]=2[CH:3]=1.C(N(CC)CC)C.[C:25](Br)(=[O:27])[CH3:26]>C(Cl)Cl>[C:25]([N:10]1[C:11]2[CH2:12][CH2:13][C:4]3[CH:3]=[C:2]([Cl:1])[CH:17]=[CH:16][C:5]=3[C:6]=2[C:7]([CH3:14])([CH3:15])[CH2:8][CH2:9]1)(=[O:27])[CH3:26]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 10482Acetyl bromideHCID 198331288-Chloro-1,1-dimethyl-1,2,3,4,5,6-hexahydrobenzo[f]quinoline

생성물 1

HCID 198331574-Acetyl-8-chloro-1,1-dimethyl-1,2,3,4,5,6-hexahydrobenzo[f]quinoline

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

10.6 g (0.043 mol) of 8-chloro-1,1-dimethyl -1,2,3,4,5,6-hexahydrobenzo[f]quinoline and 6.6 ml (0.047 mol) of triethylamine are dissolved in 100 ml of methylene chloride and 3.5 ml (0.047 mol) of acetyl bromide dissolved in 20 ml of methylene chloride are added dropwise thereto at 0°. After stirring for 1 hour, the mixture is extracted with methylene chloride/water, dried with magnesium sulfate and the solvent is distilled in a vacuum. Recrystallization from methylene chloride/ hexane gives 4-acetyl-8-chloro-1,1-dimethyl-1,2,3,4,5,6hexahydrobenzo[f]quinoline as white crystals with melting point 126-127°.

후처리

  1. additionare added dropwise
  2. customat 0°
  3. extractionthe mixture is extracted with methylene chloride/water
  4. dry with materialdried with magnesium sulfate
  5. distillationthe solvent is distilled in a vacuum
  6. customRecrystallization from methylene chloride/ hexane

출처 및 근거

ORD 기록
ord-64e278da835c4172b5f5c81b9aed497f
출처 데이터셋
uspto-grants-1991_05
특허 번호
US05017608

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