Acetamidine monohydrochloride → 4-(Dimethoxymethyl)-2-methylpyrimidine

HRID 1924112

반응식

HRID 1924112 반응식
Cl.[C:2]([NH2:5])(=[NH:4])[CH3:3].CN(C)[CH:8]=[CH:9][C:10](=O)[CH:11]([O:14][CH3:15])[O:12][CH3:13].C[O-].[Na+]>CO>[CH3:13][O:12][CH:11]([O:14][CH3:15])[C:10]1[CH:9]=[CH:8][N:5]=[C:2]([CH3:3])[N:4]=1

참가 물질

5

반응물 3

HCID 67170Acetamidine monohydrochlorideHCID 27821454-(Dimethylamino)-1,1-dimethoxybut-3-en-2-oneHCID 10942334Sodium Methoxide

생성물 1

HCID 27995724-(Dimethoxymethyl)-2-methylpyrimidine수율 91.3%

시약·촉매·용매 1

HCID 887Methanol용매2회

반응 조건

온도
40 °C

실험 절차

Acetamidine hydrochloride (3 mol) and 4-dimethylamino-1,1-dimethoxy-but-3-en-2-one (2 mol) were mixed in methanol (500 ml) and the reaction mixture was warmed to 40° C. A solution of sodium methoxide in methanol (558 g, 30%) was added quickly and a brown suspension was formed. The reaction mixture was heated under reflux for 2 h, cooled to room temperature overnight followed by evaporation of methanol under reduced pressure. The resulting residue was taken up in dichloromethane (500 ml) and washed several times with water (100 mL). The solvent was removed to give 307 g of black oil. The distillation of this oil gave a colourless liquid of boiling point 55-58° C. (0.5 mbar).

후처리

  1. customa brown suspension was formed
  2. temperatureThe reaction mixture was heated
  3. temperatureunder reflux for 2 h
  4. temperaturecooled to room temperature overnight
  5. customfollowed by evaporation of methanol under reduced pressure
  6. washwashed several times with water (100 mL)
  7. customThe solvent was removed

출처 및 근거

ORD 기록
ord-e4f679468da6435e90e93b8b381cd5bc
출처 데이터셋
uspto-grants-2012_05
특허 번호
US08178540B2

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