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

HRID 1845858ノート

反応式

HRID 1845858 の反応式
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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-f41f0e4475744640919d6cedb81c4085
出典データセット
uspto-grants-2015_02
特許番号
US08952001B2

反応ノート

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