Sodium Methoxide → 2-Butyl-6-(2,2-dimethyl-1-oxopropyl)-5,6,7,8-tetrahydro-pyrido[4,3-d]pyrimidin-4(3H)-one

HRID 1198461

반응식

HRID 1198461 반응식
[CH3:1][C:2]([CH3:18])([CH3:17])[C:3]([N:5]1[CH2:10][CH2:9][C:8](=O)[CH:7]([C:12]([O:14]CC)=O)[CH2:6]1)=[O:4].Cl.[C:20]([NH2:26])(=[NH:25])[CH2:21][CH2:22][CH2:23][CH3:24].C[O-].[Na+]>C(O)C.CO>[CH2:21]([C:20]1[NH:26][C:12](=[O:14])[C:7]2[CH2:6][N:5]([C:3](=[O:4])[C:2]([CH3:1])([CH3:17])[CH3:18])[CH2:10][CH2:9][C:8]=2[N:25]=1)[CH2:22][CH2:23][CH3:24]

참가 물질

6

반응물 3

HCID 10942334Sodium MethoxideHCID 11615174Pentanimidamide HydrochlorideHCID 19102683Ethyl 1-(2,2-dimethyl-1-oxopropyl)-4-oxo-3-piperidinecarboxylate

생성물 1

HCID 1356749702-Butyl-6-(2,2-dimethyl-1-oxopropyl)-5,6,7,8-tetrahydro-pyrido[4,3-d]pyrimidin-4(3H)-one수율 67.4%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 887Methanol용매

실험 절차

A mixture of 1.3 g of ethyl 1-(2,2-dimethyl-1-oxopropyl)-4-oxo-3-piperidinecarboxylate and 0.75 g of valeramidine hydrochloride in 10 ml of anhydrous ethyl alcohol is treated with 5.3 ml of a 1M solution of sodium methoxide in methanol. The resulting mixture is stirred and heated at reflux for one hour. The reaction mixture is allowed to cool over 30 minutes then filtered. The filtrate is evaporated to a gummy residue and stirred with 40 ml of ether for 30 minutes, filtered and the cake washed with ether. The cake is dried at 56° C. under vacuum to afford 1.0 g of the desired product as a colorless solid, m.p. 167°-172° C.

후처리

  1. temperatureheated
  2. temperatureat reflux for one hour
  3. temperatureto cool over 30 minutes
  4. filtrationthen filtered
  5. customThe filtrate is evaporated to a gummy residue
  6. stirringstirred with 40 ml of ether for 30 minutes
  7. filtrationfiltered
  8. washthe cake washed with ether
  9. customThe cake is dried at 56° C. under vacuum

출처 및 근거

ORD 기록
ord-b184e56a4caf4599a1d7f0c6a1db0177
출처 데이터셋
uspto-grants-1994_01
특허 번호
US05281602

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