Sodium hydride → HCID 385279, 화합물

반응식

[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

참가 물질

반응물 4

HCID 24758Sodium hydride

HCID 312751,4-Dioxane2회

HCID 655222-Amino-4,6-dichloropyrimidine

HCID 17797766HCID 17797766, 화합물

생성물 1

HCID 385279HCID 385279, 화합물수율 50.8%

반응 조건

온도: 65 °C

실험 절차

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).