반응 #220422

반응 방정식

sodium hydride

5,7-dihydro-6H-dibenz[b,d]azepin-6-one

methyl iodide

→

title compound

수율 63.7%

7-Methyl-5,7-dihydro-6H-dibenz[b,d]azepin-6-one

수율 63.7%

용매

DMF

CH2Cl2 H2O

반응 조건

후처리

1. 1
   기타prepared
2. 2
   workup.STIRRINGstirring
3. 3
   workup.WAITcontinued for 17 h with the exclusion of light
4. 4
   온도After cooling
5. 5
   세척washed with NaHSO4 solution, H2O
6. 6
   건조dried over Na2SO4
7. 7
   기타Evaporation and flash chromatography (SiO2, CHCl3)

실험 절차

A round bottom flask was charged with sodium hydride (0.295 g, 7.46 mmol) in 9.0 ml of DMF and treated with 5,7-dihydro-6H-dibenz[b,d]azepin-6-one (1.3 g, 6.22 mmol) (CAS #20011-90-9, prepared as described in Brown, et. al., Tetrahedron Letters, No. 8, 667-670, (1971) and references cited therein). After stirring at 60° C. for 1 h, the solution was treated with methyl iodide (1.16 ml, 18.6 mmol) and stirring continued for 17 h with the exclusion of light. After cooling, the reaction was diluted with CH2Cl2/H2O, washed with NaHSO4 solution, H2O, and dried over Na2SO4. Evaporation and flash chromatography (SiO2, CHCl3) gave 0.885 g (63%) of the title compound as a colorless solid.

출처