反応 #75051

反応方程式

homoveratrylamine

β-phenethyl bromide

→

N-phenethyl-3,4-dimethoxyphenethylamine hydrobromide

収率 44.5%

溶媒

acetone

反応条件

後処理

1. 1
   温度after cooling the mixture to 60° C.
2. 2
   ろ過vacuum filtered
3. 3
   workup.DISSOLUTIONthe recovered precipitate was dissolved in 250 ml of methanol
4. 4
   濃縮The solution was concentrated to 50 ml and 400 ml of ethyl acetate
5. 5
   workup.ADDITIONwere added
6. 6
   濃縮The mixture was concentrated to 200 ml
7. 7
   ろ過vacuum filtered
8. 8
   その他to obtain 12.5 g of raw product
9. 9
   その他The latter was crystallized from isopropanol

実験手順

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.

出典