反应详情

A mixture of 18 ml of 40% aqueous dimethylamine solution and 19.8 ml of acetic acid is treated with 9 ml of 37% formalin at 10° - 15° C. The resulting solution is added at once to 10 g of 4,4-dimethyl-4H-pyrrolo[2,1-c][1,4]benzoxazine (10. g, described in Example 78) in 30 ml of ethanol. The reaction mixture is stirred at ambient temperature for 18 hr. Ethanol is removed under reduced pressure, and the remaining oily suspension is extracted with chloroform. The combined extracts are dried (Na2SO4), filtered, and evaporated to yield the title compound, nmr (CDCl3) δ 1.56 (s, 6H), 2.67 (d, J = 4.5Hz, 6H), 4.70 (d, J = 4.5Hz, 2H), 6.08 and 6.85 (d, 2H), 6.95 - 7.70 (m, 4H), 12.4 (broad, 1H).

1. customEthanol is removed under reduced pressure
2. extractionthe remaining oily suspension is extracted with chloroform
3. dry with materialThe combined extracts are dried (Na2SO4)
4. filtrationfiltered
5. customevaporated