Sodium Hydroxide → N-(3-(1H-Imidazol-1-yl)phenyl)-4-(2-pyridinyl)-2-pyrimidinamine

HRID 973801

反応式

HRID 973801 の反応式
Cl.Cl.[N:3]1([C:8]2[CH:9]=[C:10]([NH:14][C:15]([NH2:17])=[NH:16])[CH:11]=[CH:12][CH:13]=2)[CH:7]=[CH:6][N:5]=[CH:4]1.CN(C)[CH:20]=[CH:21][C:22]([C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][N:25]=1)=O.[OH-].[Na+]>C(O)CC>[N:3]1([C:8]2[CH:9]=[C:10]([NH:14][C:15]3[N:17]=[C:22]([C:24]4[CH:29]=[CH:28][CH:27]=[CH:26][N:25]=4)[CH:21]=[CH:20][N:16]=3)[CH:11]=[CH:12][CH:13]=2)[CH:7]=[CH:6][N:5]=[CH:4]1

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 5669933-Dimethylamino-1-(2-pyridyl)prop-2-en-1-oneHCID 178478791[3-(1H-Imidazol-1-yl)phenyl]guanidine, dihydrochloride

生成物 1

HCID 163890N-(3-(1H-Imidazol-1-yl)phenyl)-4-(2-pyridinyl)-2-pyrimidinamine収率 85%

試薬・触媒・溶媒 1

HCID 10311-Propanol溶媒2 回

実験手順

Thirteen and seven tenths grams of [3-(1H-imidazol-1-yl)phenyl]guanidine, dihydrochloride (2) from Example 1, 8.8 g of 3-dimethylamino-1-(2-pyridyl)-2-propen-1-one (3), 50 ml of n-propanol and 10 ml of 10N sodium hydroxide is refluxed for 18 hours. The reaction is diluted with 50 ml of n-propanol and filtered. The collected yellow solid is stirred in 300 ml of water for 0.5 hour, filtered and washed with 50 ml of n-propanol followed by 100 ml of diethyl ether. The solid is air dried overnight giving 13.4 g (85%) of the desired product, mp 210°-211° C. The overall yield following this procedure is 73%.

後処理

  1. filtrationfiltered
  2. filtrationfiltered
  3. washwashed with 50 ml of n-propanol
  4. customdried overnight

出典と根拠

ORDレコード
ord-f7a7a792e05042bd8c3706df6930a809
出典データセット
uspto-grants-1991_11
特許番号
US05064963

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