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CH 150 → 2,6-dimethyl-3-ethyl-4-oxo-6,7,8,9-tetrahydro-4H-pyrido(1,2-a)pyrimidine

HRID 1578096
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반응식

HRID 1578096 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]>C(O)C>[CH3:1][C:2]1[N:3]=[C:4]2[CH2:14][CH2:13][CH2:12][CH:11]([CH3:15])[N:5]2[C:6](=[O:10])[C:7]=1[CH2:8][CH3:9]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 1

HCID 93406CH 150

생성물 1

HCID 125274322,6-dimethyl-3-ethyl-4-oxo-6,7,8,9-tetrahydro-4H-pyrido(1,2-a)pyrimidine수율 99.5%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

4.04 g. of 2,6-dimethyl-3-ethyl-4-oxo-4H-pyrido(1,2-a)pyrimidine are dissolved in 50 ml. of ethanol and the solution is hydrogenated in the presence of 2 g. of Raney-nickel catalyst, previously washed to anhydrous with ethanol. Hydrogenation is performed under atmospheric pressure. In about seven hours the calculated amount of hydrogen is used up and the hydrogen consumption drops rapidly to zero. The catalyst is filtered off and the ethanol solution is evaporated. 4.10 g. (99.5%) of 2,6-dimethyl-3-ethyl-4-oxo-6,7,8,9-tetrahydro-4H-pyrido(1,2-a)pyrimidine are obtained as a pale-yellow non-crystallizing oil, which can be distilled under a pressure of 25 mmHg of 190° C.

후처리

  1. washof Raney-nickel catalyst, previously washed to anhydrous with ethanol
  2. customthe hydrogen consumption
  3. filtrationThe catalyst is filtered off
  4. customthe ethanol solution is evaporated

출처 및 근거

ORD 기록
ord-164a4b1797dd4b5aa60608e4e52c063a
출처 데이터셋
uspto-grants-1981_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04291036

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