反应详情

To a mixture of 2-ethyl-6-methyl-isonicotinic acid (87.9 mg, 0.53 mmol), 1,1,2-trimethyl-1,1a,5,5a-tetrahydro-3-thia-cyclopropa[a]pentalene-4-carboxylic acid hydrazide (141.8 mg, 0.6 mmol), HOBt (100 mg, 0.74 mmol) and TEA (0.42 mL) in DCM (5 mL) is added at 0° C. EDC (200 mg, 0.78 mmol). The mixture is stirred for 15 h during which time it warmed from 0° C. to rt. The mixture is quenched with EA (50 mL) and washed with 1M aq. NaOH (2×10 mL). The organic phase is dried (Na2SO4), filtered and evaporated to give crude 2-ethyl-6-methyl-isonicotinic acid N′-(1,1,2-trimethyl-1,1a,5,5a-tetrahydro-3-thia-cyclopropa[a]pentalene-4-carbonyl)-hydrazide (350 mg); LC-MS: tR=0.80 min, [M+1]=384.34.

1. additionis added at 0° C
2. temperaturewarmed from 0° C. to rt
3. customThe mixture is quenched with EA (50 mL)
4. washwashed with 1M aq. NaOH (2×10 mL)
5. dry with materialThe organic phase is dried (Na2SO4)
6. filtrationfiltered
7. customevaporated