Sodium Carbonate → 5-Amino-5-methylheptan-3-one
반응식
C(C1(C)N=[C:7]([CH2:9][CH3:10])[CH2:6][C:5]([CH2:12][CH3:13])([CH3:11])[NH:4]1)C.C(=O)([O-])[O-:16].[Na+].[Na+]>Cl>[NH2:4][C:5]([CH3:11])([CH2:12][CH3:13])[CH2:6][C:7](=[O:16])[CH2:9][CH3:10]참가 물질
4
실험 절차
196.3 g of 2,4,6-triethyl-2,6-dimethyl-1,2,5,6-tetrahydropyrimidine were added dropwise to 300 ml of concentrated hydrochloric acid at 30° - 40° C, with stirring. When the addition was complete, the mixture was stirred for a further 4 - 5 hours and then neutralized with sodium carbonate and extracted with benzene. The resulting benzene solution was washed with, in turn, a 5% aqueous solution of sodium carbonate and water, and was then dried over potassium carbonate. After removal of benzene, the residue was distilled under reduced pressure, giving 72.4 g of 5-amino-5-methyl-3-heptanone (bp 46° - 48° C/2.5 mmHg).
후처리
- additionWhen the addition
- stirringthe mixture was stirred for a further 4 - 5 hours
- extractionextracted with benzene
- washThe resulting benzene solution was washed with, in turn
- dry with materiala 5% aqueous solution of sodium carbonate and water, and was then dried over potassium carbonate
- customAfter removal of benzene
- distillationthe residue was distilled under reduced pressure
출처 및 근거
- ORD 기록
- ord-26d4840fd9a34dd684296857809976ea
- 출처 데이터셋
- uspto-grants-1978_06
- 특허 번호
- US04097587
반응 노트
불러오는 중…