반응 #2078470

반응 방정식

3,4-dihydro-7-nitro-2H-1,4-benzothiazin-3-one

potassium carbonate

Water

iodomethane

→

title compound

수율 90.0%

3,4-dihydro-4-methyl-7-nitro-2H-1,4-benzothiazin-3-one

수율 90.0%

용매

DMF

반응 조건

후처리

1. 1
   온도to cool down
2. 2
   여과the precipitate is filtered off
3. 3
   세척washed with water (10 mL)
4. 4
   기타The resulting solid is dried under high vacuum

실험 절차

To a stirred suspension of 3,4-dihydro-7-nitro-2H-1,4-benzothiazin-3-one (Step 2, 4.7 g, 22.3 mmol) and potassium carbonate (3.70 g, 26.8 mmol) in dry DMF (40 mL) in an ice bath is added iodomethane (4.16 mL, 66.8 mmol). The reaction mixture is taken out of the ice bath and heated at 50° C. for 1-2 h. The resulting mixture is allowed to cool down. Water (35 mL) and ice are added and the precipitate is filtered off and washed with water (10 mL). The resulting solid is dried under high vacuum to give the title compound as a yellow solid (4.5 g, 90%), MS m/z 225.5 (M+H)+.

출처