Sodium hydride → HCID 385279、化合物

反応式

[H-].[Na+].O[CH:4]([CH:6]1[CH2:9][CH2:8][CH2:7]1)[OH:5].[NH2:10][C:11]1[N:16]=[C:15](Cl)[CH:14]=[C:13]([Cl:18])[N:12]=1.[O:19]1CCOC[CH2:20]1>>[NH2:10][C:11]1[N:16]=[C:15]([O:5][CH2:4][C:6]2([CH2:20][OH:19])[CH2:9][CH2:8][CH2:7]2)[CH:14]=[C:13]([Cl:18])[N:12]=1

参加物

反応物 4

HCID 24758Sodium hydride

HCID 312751,4-Dioxane2 回

HCID 655222-Amino-4,6-dichloropyrimidine

HCID 17797766HCID 17797766、化合物

生成物 1

HCID 385279HCID 385279、化合物収率 50.8%

反応条件

温度: 65 °C

実験手順

60% Sodium hydride (0.4 g, 0.01 mol) was suspended in dry dioxane (40 ml) and dihydroxymethylcyclobutane (1.16 g, 0.01 mol) dissolved in dry dioxane (40 ml) was dropwise added thereto. The mixture was stirred at 60-70° C. for 30 minutes, and 2-amino-4,6-dichloropyrimidine (1.64 g, 0.01 mol) was added. The mixture was refluxed for 3 hours, and filtrated. The solvent in the filtrate was distilled away under reduced pressure and the residue was purified by silica gel column chromatography (chloroform:methanol=50:1) to give white crystals (1.24 g, 50.8%), m.p. 125-127° C. (acetone).