Water → Acryloyl-1-cyclohexyl-1,2,3,4-tetrahydroisoquinoline

HRID 2383013노트

반응식

HRID 2383013 반응식
Cl.[CH:2]1([CH:8]2[C:17]3[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=3)[CH2:11][CH2:10][NH:9]2)[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3]1.O.[C:19](Cl)(=[O:22])[CH:20]=[CH2:21]>C(Cl)Cl.C(N(CC)CC)C>[C:19]([C:8]1([CH:2]2[CH2:3][CH2:4][CH2:5][CH2:6][CH2:7]2)[C:17]2[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=2)[CH2:11][CH2:10][NH:9]1)(=[O:22])[CH:20]=[CH2:21]

참가 물질

6

반응물 3

HCID 962WaterHCID 13140Acryloyl chlorideHCID 675358401-Cyclohexyl-1,2,3,4-tetrahydroisoquinoline hydrochloride

생성물 1

HCID 70661750Acryloyl-1-cyclohexyl-1,2,3,4-tetrahydroisoquinoline

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 8471Triethylamine용매

실험 절차

1-cyclohexyl-1,2,3,4-tetrahydroisoquinoline hydrochloride (800 mg) was dissolved in methylene chloride (12 mL), to which triethylamine (1.1 mL) and acryloyl chloride (0.28 mL) were then added under ice-cooling, followed by stirring under ice-cooling for 30 minutes and then stirring at room temperature for 14 hours. Water was added to the reaction liquid which was then extracted with chloroform. The extract was washed with saturated brine and dried over magnesium sulfate. The solvent was evaporated to obtain 2 acryloyl-1-cyclohexyl-1,2,3,4-tetrahydroisoquinoline (856 mg).

후처리

  1. additionwere then added under ice-
  2. temperaturecooling
  3. temperaturecooling for 30 minutes
  4. stirringstirring at room temperature for 14 hours
  5. extractionwas then extracted with chloroform
  6. washThe extract was washed with saturated brine
  7. dry with materialdried over magnesium sulfate
  8. customThe solvent was evaporated

출처 및 근거

ORD 기록
ord-1222394dbe614dbab8e745e9ce1ab195
출처 데이터셋
uspto-grants-2012_09
특허 번호
US08263607B2

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