Acetone → 1,2,6-trimethyl-3-ethyl-1,2,3,6,7,8,9,9a-octahydro-4-oxo-4H-pyrido(1,2-a)pyrimidine hydrochloride
반응식
[CH3:1][C:2]1[N:3]=[C:4]2[CH:14]=[CH:13][CH:12]=[C:11]([CH3:15])[N:5]2[C:6](=[O:10])[C:7]=1[CH2:8][CH3:9].[CH3:16]C(C)=O.CI.[ClH:22]>C(O)C.O>[ClH:22].[CH3:16][N:3]1[CH:2]([CH3:1])[CH:7]([CH2:8][CH3:9])[C:6](=[O:10])[N:5]2[CH:11]([CH3:15])[CH2:12][CH2:13][CH2:14][CH:4]12참가 물질
실험 절차
0.01 moles of 2,6-dimethyl-3-ethyl-4-oxo-4H-pyrido(1,2-a)pyrimidine are dissolved in 20 ml. of acetone, 0.03 moles of methyl iodide are added and the mixture is kept in a bomb tube at 150° C. for 24 hours. The solution is evaporated to dryness, the residue is dissolved in 15 ml. of methanol and a solution of 0.05 moles of sodium tetrahydroborate(III) in 10 ml. of water is added. After 4 hours the methanol is distilled off and the aqueous phase is extracted with three 20-ml. portions of chloroform. The organic phase is dried, evaporated and added to the oily substance obtained are 10 ml. of ethanol saturated with hydrochloric acid. 1,2,6-trimethyl-3-ethyl-1,2,3,6,7,8,9,9a-octahydro-4-oxo-4H-pyrido(1,2-a)pyrimidine hydrochloride is obtained, while crystallizes when triturated with ether. The product obtained after recrystallization from a mixture of acetone and ether sublimates over 206° C. Yield: 41%.
후처리
- customThe solution is evaporated to dryness
- dissolutionthe residue is dissolved in 15 ml
- distillationAfter 4 hours the methanol is distilled off
- extractionthe aqueous phase is extracted with three 20-ml
- customThe organic phase is dried
- customevaporated
- additionadded to the oily substance
- customobtained
출처 및 근거
- ORD 기록
- ord-cdff470511984834a49abfcc9e53c1ca
- 출처 데이터셋
- uspto-grants-1981_09
- 특허 번호
- US04291036
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