Guanidine Hydrochloride → 4-(1,1-Dimethoxyethyl)pyrimidin-2-amine

HRID 1845858노트

반응식

HRID 1845858 반응식
CN(C)[CH:3]=[CH:4][C:5](=O)[C:6]([O:10][CH3:11])([O:8][CH3:9])[CH3:7].C(=O)([O-])[O-].[K+].[K+].Cl.[NH2:21][C:22]([NH2:24])=[NH:23]>C(O)C>[CH3:9][O:8][C:6]([C:5]1[CH:4]=[CH:3][N:21]=[C:22]([NH2:24])[N:23]=1)([O:10][CH3:11])[CH3:7]

참가 물질

5

반응물 3

HCID 5742Guanidine HydrochlorideHCID 11430Potassium CarbonateHCID 5668111-Penten-3-one, 1-(dimethylamino)-4,4-dimethoxy-

생성물 1

HCID 135822684-(1,1-Dimethoxyethyl)pyrimidin-2-amine수율 62.6%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

1-(dimethylamino)-4,4-dimethoxypent-1-en-3-one (1a) (34.29 g) was dissolved in ethanol (750 mL). Potassium carbonate (65.3 g) and guanidine hydrochloride (20.77 g) were added and the resulting suspension heated to reflux overnight. The reaction mixture was concentrated in vacuo, the residue was stirred with water overnight, filtered and dried in a vacuum oven at 40° C. overnight to afford the title compound (21.01 g) as a white solid. The filtrate was extracted with dichloromethane (3×700 mL) and the combined organic layers were dried over sodium sulfate and concentrated in vacuo to afford a further crop (10.6 g) of the title compound.

후처리

  1. temperaturethe resulting suspension heated
  2. temperatureto reflux overnight
  3. concentrationThe reaction mixture was concentrated in vacuo
  4. filtrationfiltered
  5. customdried in a vacuum oven at 40° C. overnight

출처 및 근거

ORD 기록
ord-f41f0e4475744640919d6cedb81c4085
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08952001B2

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