反应详情

To a solution of 2-isobutyl-6-methyl-isonicotinic acid (83 mg, 0.359 mmol) and DIPEA (186 mg, 1.44 mmol) in DMF (6 mL) is added TBTU (127 mg, 0.395 mmol) at rt. The mixture is stirred for 45 min before 1 M hydrazine in THF (1.44 mL, 1.44 mmol) is added and stirring is continued for 2 h. The mixture is diluted with ether (200 mL) and washed with 1M aq. HCl (3×5 mL), 1M aq. NaOH (3×5 mL) and brine (5 mL). The org. phase is separated, dried over MgSO4, filtered and evaporated. The crude product is purified on prep. TLC plates with DCM containing 4% of methanol to give 2-isobutyl-6-methyl-isonicotinic acid hydrazide (37 mg) as a yellow oil; LC-MS: tR=0.44 min, [M+1]+=208.10.

1. additionis added
2. washwashed with 1M aq. HCl (3×5 mL), 1M aq. NaOH (3×5 mL) and brine (5 mL)
3. customphase is separated
4. dry with materialdried over MgSO4
5. filtrationfiltered
6. customevaporated
7. customThe crude product is purified on prep