β-溴苯乙烷 → 2-(3,4-Dimethoxyphenyl)-N-(2-phenylethyl)ethan-1-amine--hydrogen bromide (1/1)

HRID 46773

反应方程式

HRID 46773 反应方程式
[CH2:1]([NH2:13])[CH2:2][C:3]1[CH:12]=[CH:11][C:8]([O:9][CH3:10])=[C:5]([O:6][CH3:7])[CH:4]=1.[CH:14]1[CH:19]=[CH:18][C:17]([CH2:20][CH2:21][Br:22])=[CH:16][CH:15]=1>CC(C)=O>[BrH:22].[CH2:21]([NH:13][CH2:1][CH2:2][C:3]1[CH:12]=[CH:11][C:8]([O:9][CH3:10])=[C:5]([O:6][CH3:7])[CH:4]=1)[CH2:20][C:17]1[CH:18]=[CH:19][CH:14]=[CH:15][CH:16]=1

参与物

4

反应物 2

HCID 7666β-溴苯乙烷HCID 84213,4-二甲氧基苯乙胺

产物 1

HCID 30486862-(3,4-Dimethoxyphenyl)-N-(2-phenylethyl)ethan-1-amine--hydrogen bromide (1/1)收率 44.5%

试剂、催化剂与溶剂 1

HCID 180丙酮溶剂

反应条件

温度
125 °C

实验过程

A mixture of 10 g of homoveratrylamine and 12 g of β-phenethyl bromide was stirred for 15 minutes at 125° C. in a bath and after cooling the mixture to 60° C., 30 ml of acetone were added. The mixture was iced and vacuum filtered and the recovered precipitate was dissolved in 250 ml of methanol. The solution was concentrated to 50 ml and 400 ml of ethyl acetate were added thereto. The mixture was concentrated to 200 ml, was iced and vacuum filtered to obtain 12.5 g of raw product. The latter was crystallized from isopropanol to obtain 9 g of N-phenethyl-3,4-dimethoxyphenethylamine hydrobromide in the form of colorless crystals melting at 180° C.

后处理

  1. temperatureafter cooling the mixture to 60° C.
  2. filtrationvacuum filtered
  3. dissolutionthe recovered precipitate was dissolved in 250 ml of methanol
  4. concentrationThe solution was concentrated to 50 ml and 400 ml of ethyl acetate
  5. additionwere added
  6. concentrationThe mixture was concentrated to 200 ml
  7. filtrationvacuum filtered
  8. customto obtain 12.5 g of raw product
  9. customThe latter was crystallized from isopropanol

来源与证据

ORD记录
ord-8fad7de4d05543a687b763c106462129
来源数据集
uspto-grants-1979_11
专利号
US04175136

关联笔记

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