Dichloromethane → HCID 23564544、化合物

反応式

[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[NH:7][CH2:8][C:9]([C:11]1[CH:12]=[CH:13][C:14]2[S:19][C:18]3[N:20]=[CH:21][CH:22]=[N:23][C:17]=3[N:16](COC)[C:15]=2[CH:27]=1)=O.S(Cl)(Cl)=O.ClCCl>C(Cl)(Cl)(Cl)Cl>[N:7]1[CH:8]=[C:9]([C:11]2[CH:12]=[CH:13][C:14]3[S:19][C:18]4[N:20]=[CH:21][CH:22]=[N:23][C:17]=4[NH:16][C:15]=3[CH:27]=2)[N:1]2[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=12

参加物

実験手順

10 ml of a solution of 200 mg of [N-(2-pyridyl)aminometyl](10-methoxymethyl-10H-pyrazino[2,3-b][1,4]benzothiazin-8-yl)ketone in carbon tetrachloride was stirred at room temperature and 240 mg of thionyl chloride was dropped thereinto. The reaction mixture was distributed into dichloromethane and an aqueous solution of sodium bicarbonate and the organic layer was separated. To the organic layer were added methanol and tetrahydrofuran to give a homogeneous solution. After adding silica gel and distilling off the solvent under reduced pressure, the residue was purified by silica gel column chromatography (eluted with dichloromethane/methanol) to thereby give 103 mg of the title compound as yellow crystals.