Methanol → 3-Ethyl-7,8-dimethoxy-1-phenyl-2,3,4,5-tetrahydro-1H-3-benzazepine

HRID 972349ノート

反応式

HRID 972349 の反応式
[CH3:1][O:2][C:3]1[C:19]([O:20][CH3:21])=[CH:18][C:6]2[CH:7]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=3)[CH2:8][NH:9][CH2:10][CH2:11][C:5]=2[CH:4]=1.[CH2:22](Br)[CH3:23].[OH-].[K+].CO>C(OCC)(=O)C>[CH3:1][O:2][C:3]1[C:19]([O:20][CH3:21])=[CH:18][C:6]2[CH:7]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=3)[CH2:8][N:9]([CH2:22][CH3:23])[CH2:10][CH2:11][C:5]=2[CH:4]=1

参加物

6

反応物 4

HCID 887MethanolHCID 6332Ethyl BromideHCID 14797Potassium HydroxideHCID 105409631H-3-Benzazepine, 2,3,4,5-tetrahydro-7,8-dimethoxy-1-phenyl-

生成物 1

HCID 214066873-Ethyl-7,8-dimethoxy-1-phenyl-2,3,4,5-tetrahydro-1H-3-benzazepine

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

A sample of 7,8-dimethoxy-1-phenyl-2,3,4,5,-tetrahydro-1H-3-benzazepine weighing 4.32 g. (0.0154 mol), 2.18 g. (0.02 mol) of ethyl bromide and 1.12 g. (0.02 mol) of potassium hydroxide are dissolved in 120 ml. of dry methanol and the solution is refluxed overnight. Evaporation of the solution to dryness gives a mixture which is taken up in ethyl acetate and filtered to remove inorgaic salts. The filtrate is washed with water, dried and evaporated to give 7,8-dimethoxy-3-ethyl-1-phenyl-2,3,4,5-tetrahydro-1H-3-benzazepine as an oil.

後処理

  1. customEvaporation of the solution to dryness
  2. customgives a mixture which
  3. filtrationfiltered
  4. customto remove inorgaic salts
  5. washThe filtrate is washed with water
  6. customdried
  7. customevaporated

出典と根拠

ORDレコード
ord-0eef670453494b7bb628cf3fcf679a1e
出典データセット
uspto-grants-1977_10
特許番号
US04052506

反応ノート

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