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

HRID 2383013ノート

反応式

HRID 2383013 の反応式
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]

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 8471Triethylamine溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-1222394dbe614dbab8e745e9ce1ab195
出典データセット
uspto-grants-2012_09
特許番号
US08263607B2

反応ノート

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