تفاعل #2045093
ord-457ecc6eabfb4774b861b707817d9960
معادلة التفاعل
2-bromo-1-(4-chlorophenyl)ethanone
acetonitrile
→
2-amino-1-(4-chlorophenyl)ethanone hydrochloride
المردود 50.0%
الكواشف
لا شيء
ظروف التفاعل
درجة الحرارة
105°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1درجة الحرارةwas heated
- 2أخرىThe formed sodium bromide was removed by filtration
- 3تركيزthe filtrate concentrated in vacuo
- 4workup.DISSOLUTIONThe residue was dissolved in ethanol (2.5 mL per mmol)
- 5workup.ADDITIONconc. aq. hydrochloric acid (0.9 mL per mmol) added at ambient temperature
- 6ترشيحwere filtered off
- 7غسيلwashed with ethanol (1×0.5 mL per mmol)
- 8أخرىDrying of the solids
الإجراء التجريبي
A mixture of 2-bromo-1-(4-chlorophenyl)ethanone (1.0 eq.) and NaN(CHO)2 (1.1 eq.) in acetonitrile (1.5 mL per mmol) was heated to reflux for 4 h at 105° C. ext. temperature. The formed sodium bromide was removed by filtration and the filtrate concentrated in vacuo. The residue was dissolved in ethanol (2.5 mL per mmol) and conc. aq. hydrochloric acid (0.9 mL per mmol) added at ambient temperature. After stirring for 72 h at room temperature the solids were filtered off and washed with ethanol (1×0.5 mL per mmol). Drying of the solids afforded 2-amino-1-(4-chlorophenyl)ethanone hydrochloride in ca. 50% yield that was used in the next step without purification.