反应详情

A mixture of N-[(1,3,4,9-tetrahydro-1-methylpyrano[3,4-b]indol-1-yl)methyl]-acetamide (2.7 g, described in Example 1), phosphorus oxychloride (1.8 ml) and dry benzene (150 ml) is stirred and refluxed for 2 hours, cooled and washed with water (10° C.). The aqueouslayer is separated, basified with 5N sodium hydroxide, and extracted with chloroform. The combined organic extracts are dried over magnesium sulfate, filtered and evaporated to give a residue of the title compound. The residue is dissolved in diethyl ether and hydrogen chloride is added until precipitation is completed. The precipitate is collected and crystallized from ethanol-diethyl ether to obtain the hydrochloride salt of the title compound (1.45 g); mp 226°-227° C.; ir(CHCl3) 2500, 1815, 1623, 1536, 1662 and 1575 cm-1 ; mr (CDCI3) δ 1.66 (s), 2.90 (m), 3.32 (s), 3,48 (d), 4.30 (m) and 7.51 (m).

1. temperaturerefluxed for 2 hours
2. temperaturecooled
3. washwashed with water (10° C.)
4. customThe aqueouslayer is separated
5. extractionextracted with chloroform
6. dry with materialThe combined organic extracts are dried over magnesium sulfate
7. filtrationfiltered
8. customevaporated