反応 #432716

反応方程式

2,6-dichlorobenzoyl chloride

2-chloroethanamine hydrochloride

potassium carbonate

water

→

2,6-dichloro-N-(2-chloroethyl)benzamide

収率 68.8%

溶媒

dichloromethane

反応条件

後処理

1. 1
   workup.ADDITIONwas added dropwise
2. 2
   その他slightly exothermic reaction
3. 3
   workup.STIRRINGUpon completion, stirring at room temperature
4. 4
   その他The organic phase was separated
5. 5
   抽出the aqueous phase was extracted with dichloromethane
6. 6
   洗浄The combined organic phases were washed with water
7. 7
   その他dried
8. 8
   ろ過filtered
9. 9
   その他evaporated
10. 10
    その他The residue was crystallized from methylbenzene
11. 11
    ろ過The product was filtered off
12. 12
    その他dried

実験手順

To a stirred (vigorously) mixture of 17.4 parts of 2-chloroethanamine hydrochloride, 20.7 parts of potassium carbonate and 225 parts of water was added dropwise a mixture of 31.3 parts of 2,6-dichlorobenzoyl chloride and 120 parts of dichloromethane at room temperature: slightly exothermic reaction. Upon completion, stirring at room temperature was continued for one hour. The organic phase was separated and the aqueous phase was extracted with dichloromethane. The combined organic phases were washed with water, dried, filtered and evaporated. The residue was crystallized from methylbenzene. The product was filtered off and dried, yielding 25.8 parts (68.8%) of 2,6-dichloro-N-(2-chloroethyl)benzamide; mp. 113.8° C. (intermediate 30).

出典