Triethylamine → HCID 20407006, 화합물
반응식
[CH3:1][C:2]([C:5]1[CH:9]=[C:8]([NH2:10])[O:7][N:6]=1)([CH3:4])[CH3:3].C(N(CC)CC)C.[CH3:18][CH:19]([CH2:23][CH2:24][Cl:25])[C:20](Cl)=[O:21]>C(OCC)(=O)C>[Cl:25][CH2:24][CH2:23][CH:19]([CH3:18])[C:20]([NH:10][C:8]1[O:7][N:6]=[C:5]([C:2]([CH3:4])([CH3:3])[CH3:1])[CH:9]=1)=[O:21]참가 물질
5
실험 절차
To a stirred solution of 7 g of 3-(1,1-dimethylethyl)-5-aminoisoxazole dissolved in 50 ml ethyl acetate was added 5.05 g of triethylamine at room temperature. As the solution continued to stir, 8 g of 2-methyl-4-chlorobutyric acid chloride was added to the reaction mixture over a 15 minute period. The reaction was allowed to stir for about 3 days and the precipitated triethylamine hydrochloride salt was collected by filtration and washed with ethyl acetate. The solvent was evaporated from the filtrate under reduced pressure and the residue was recrystallized from diethyl ether to afford 4-chloro-N-[3-(1,1-dimethylethyl)-5-isoxazolyl]-2-methylbutanamide as a solid. mp 135°-137° C.
후처리
- stirringto stir for about 3 days
- filtrationthe precipitated triethylamine hydrochloride salt was collected by filtration
- washwashed with ethyl acetate
- customThe solvent was evaporated from the filtrate under reduced pressure
- customthe residue was recrystallized from diethyl ether
출처 및 근거
- ORD 기록
- ord-148b9ed18c734c2f92180adc2ac95b53
- 출처 데이터셋
- uspto-grants-1985_02
- 특허 번호
- US04500343
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