Diethyl 2-(p-tolyl)malonate → 5-(4-Methylphenyl)-4,6-dihydroxy-2-n-propylpyrimidine

HRID 1082313노트

반응식

HRID 1082313 반응식
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([C:14]([O:16]CC)=O)[C:9]([O:11]CC)=O)=[CH:4][CH:3]=1.Cl.[C:20]([NH2:25])(=[NH:24])[CH2:21][CH2:22][CH3:23].C[O-].[Na+]>CO>[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[C:9]([OH:11])=[N:24][C:20]([CH2:21][CH2:22][CH3:23])=[N:25][C:14]=2[OH:16])=[CH:6][CH:7]=1

참가 물질

5

반응물 3

HCID 570878Diethyl 2-(p-tolyl)malonateHCID 10942334Sodium MethoxideHCID 12828983Butanimidamide hydrochloride

생성물 1

HCID 1784184665-(4-Methylphenyl)-4,6-dihydroxy-2-n-propylpyrimidine수율 56.1%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of diethyl (4-methylphenyl)malonate (9.45 g) and butyramidine hydrochloride (5.00 g) in methanol (25 ml) is added 28% sodium methoxide (19.67 g) under ice-cooling, and the mixture is stirred at room temperature overnight. After the reaction is complete, the reaction solution is concentrated to the half volume thereof, and the resultant is diluted with water. The mixture is acidified with 10% hydrochloric acid, and the precipitated crystals are collected by filtration, washed, and dried to give 5-(4-methylphenyl)-4,6-dihydroxy-2-n-propylpyrimidine (5.17 g) as crystalline powder.

후처리

  1. temperaturecooling
  2. concentrationthe reaction solution is concentrated to the half volume
  3. additionthe resultant is diluted with water
  4. filtrationthe precipitated crystals are collected by filtration
  5. washwashed
  6. customdried

출처 및 근거

ORD 기록
ord-c5afd419830c46a6a30bf470ed776439
출처 데이터셋
uspto-grants-1996_12
특허 번호
US05589478

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