Sodium Methoxide → 6-Acetyl-2-butyl-5,6,7,8-tetrahydro-pyrido-[4,3-d]pyrimidin-4(3H)-one

HRID 1198463

반응식

HRID 1198463 반응식
[C:1]([N:4]1[CH2:9][CH2:8][C:7](=O)[CH:6]([C:11]([O:13]CC)=O)[CH2:5]1)(=[O:3])[CH3:2].Cl.[C:17]([NH2:23])(=[NH:22])[CH2:18][CH2:19][CH2:20][CH3:21].C[O-].[Na+]>C(O)C.CO>[C:1]([N:4]1[CH2:9][CH2:8][C:7]2[N:22]=[C:17]([CH2:18][CH2:19][CH2:20][CH3:21])[NH:23][C:11](=[O:13])[C:6]=2[CH2:5]1)(=[O:3])[CH3:2]

참가 물질

6

반응물 3

HCID 10942334Sodium MethoxideHCID 11615174Pentanimidamide HydrochlorideHCID 12445847Ethyl 1-acetyl-4-oxo-3-piperidinecarboxylate

생성물 1

HCID 1360140346-Acetyl-2-butyl-5,6,7,8-tetrahydro-pyrido-[4,3-d]pyrimidin-4(3H)-one수율 96.9%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 887Methanol용매

실험 절차

A mixture of 1.5 g of ethyl 1-acetyl-4-oxo-3-piperidinecarboxylate and 1.0 g of valeramidine hydrochloride in 15 ml of anhydrous ethyl alcohol is treated with 7.5 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 colorless syrup which is stirred with 50 ml of ether for 2 hours then filtered. The tacky cake is dried under high vacuum at 56° C. to afford 1.7 g of the desired product, m.p. 106°-113° 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 colorless syrup which
  6. stirringis stirred with 50 ml of ether for 2 hours
  7. filtrationthen filtered
  8. customThe tacky cake is dried under high vacuum at 56° C.

출처 및 근거

ORD 기록
ord-2c365a98f2c74fdbbaf1488ebff5bce4
출처 데이터셋
uspto-grants-1994_01
특허 번호
US05281602

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