Propanedioic acid, monoethyl ester → 2-hydroxy-7,7-dimethyl-1H,4H,6H,7H,8H-[1,3]diazino[1,2-a]pyrimidin-4-one

HRID 2408358노트

반응식

HRID 2408358 반응식
[Na].[CH3:2][C:3]1([CH3:10])[CH2:8][NH:7][C:6]([NH2:9])=[N:5][CH2:4]1.[C:11](OCC)(=[O:16])[CH2:12][C:13]([O-])=[O:14]>CO>[OH:16][C:11]1[N:9]=[C:6]2[NH:7][CH2:8][C:3]([CH3:10])([CH3:2])[CH2:4][N:5]2[C:13](=[O:14])[CH:12]=1

참가 물질

5

반응물 3

HCID 3595298Propanedioic acid, monoethyl esterHCID 5360545SodiumHCID 120527115,5-Dimethyl-1,4,5,6-tetrahydropyrimidin-2-amine

생성물 1

HCID 1363442932-hydroxy-7,7-dimethyl-1H,4H,6H,7H,8H-[1,3]diazino[1,2-a]pyrimidin-4-one수율 72%

시약·촉매·용매 1

HCID 887Methanol용매2회

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온도
100 °C

실험 절차

1.4 g of sodium are added in a fractionated way to 15 mL of MeOH. After total dissolution, 2.7 g of 5,5-dimethyl-1,4,5,6-tetrahydropyrimidin-2-amine solubilized beforehand in 5 mL of MeOH, and then 16.5 mL of ethyl malonate are added. The mixture is heated to 100° C., after 4 h of heating, the medium is dry concentrated. The obtained oil is taken up in ether. The precipitate is filtered and then the residue is taken up in 7 mL of H2O and acidified with conc. HCl up to pH 3-4. The precipitate formed is filtered, washed with ether and dried in the oven in vacuo. 2 g (yield=72%) of 2-hydroxy-7,7-dimethyl-6,7,8,9-tetrahydro-4H-pyrimido[1,2-a]pyrimidin-4-one are obtained as a beige solid used as such.

후처리

  1. temperatureof heating
  2. customthe medium is dry
  3. concentrationconcentrated
  4. filtrationThe precipitate is filtered
  5. customThe precipitate formed
  6. filtrationis filtered
  7. washwashed with ether
  8. customdried in the oven in vacuo

출처 및 근거

ORD 기록
ord-e610790dc65e4d9e9be6b9e678e2cbd2
출처 데이터셋
uspto-grants-2014_08
특허 번호
US08815853B2

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