Triethylamine → 2-bromopropionic acid N-cyano-N-butylamide
반응식
[Br:1][CH:2]([CH3:6])[C:3](Br)=[O:4].[CH2:7]([NH:11][C:12]#[N:13])[CH2:8][CH2:9][CH3:10].C(N(CC)CC)C>CCOCC>[C:12]([N:11]([CH2:7][CH2:8][CH2:9][CH3:10])[C:3](=[O:4])[CH:2]([Br:1])[CH3:6])#[N:13]참가 물질
5
실험 절차
29.5 g (0.137 mole) of 2-bromopropionyl bromide are added dropwise at 15° C. to 13.4 g (0.137 mole) of butyl cyanamide and 13.8 g (0.137 mole) of triethylamine in 150 ml of ether. The mixture is stirred for 3 hours at 20° to 25° C., then filtered to remove the precipitated salt. The filtrate is extracted with dilute hydrochloric acid and the extract is dried over sodium sulfate and concentrated by evaporation. The oily residue is distilled under high vacuum, affording 22.6 g (70.8% of theory) of 2-bromopropionic acid N-cyano-N-butylamide with a boiling point of 53°-54° C. at 0.0052 mbar.
후처리
- filtrationfiltered
- customto remove the precipitated salt
- extractionThe filtrate is extracted with dilute hydrochloric acid
- dry with materialthe extract is dried over sodium sulfate
- concentrationconcentrated by evaporation
- distillationThe oily residue is distilled under high vacuum
출처 및 근거
- ORD 기록
- ord-122e0641a6c54ab6b11527a005f8408d
- 출처 데이터셋
- uspto-grants-1988_07
- 특허 번호
- US04759796
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