3-chloro-2-methylbenzohydrazide

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: TBTU (678 mg, 2.11 mmol) was added to a rt solution of 3-chloro-2-methylbenzoic acid (300 mg, 1.76 mmol) and DIPEA (0.9 mL, 5.28 mmol) in DMF (5.0 mL) and the resulting solution was stirred at rt for 15 min. The mixture was cooled to 0° C. and 1M hydrazine in THF (10.6 mL, 10.6 mmol) was added and the yellow solution was stirred at rt overnight. The rxn mixture was diluted with DCM and washed with sat. aq. NaHCO3. The aq. layer was re-extracted with DCM (1×) and the combined org. layers were concentrated in vacuo to give the title compound D-1-2 as a light orange solid that was used further without purification. LC-MS A: tR=0.50 min; [M(35Cl)+H]+=185.24. The mixture was cooled to 0° C. the yellow solution was stirred at rt overnight washed with sat. aq. NaHCO3 The aq. layer was re-extracted with DCM (1×) layers were concentrated in vacuo