反应详情

温度

140 °C

Impure 2-methyl-propane-2-sulfinic acid[1-(6-chloro-pyridazin-3-yl)-1-methyl-ethyl]-amide (15 mg, 0.054 mmol) was combined with Pd(dppf)Cl2.dichloromethane complex (4.7 mg, 0.006 mmol), 1M K3PO4 (0.07 mL, 0.07 mmol) and 2-(hydroxymethyl)pyridine-5-boronic acid (18 mg, 0.12 mmol) in a microwave vial. A 7:3:2 mixture of DME/H2O/EtOH (1 mL) was added. The vial was flushed with argon and sealed. This vial was then heated in the microwave reactor for 15 min at 140° C. The reaction mixture was diluted with 2 mL of water and extracted 4×4 mL with EtOAc. The combined organic layers were dried over MgSO4, filtered and concentrated. Purification via normal phase flash chromatography on silica gel (0→4% MeOH/CH2Cl2) yielded 4 mg of 2-methyl-propane-2-sulfinic acid{1-[6-(6-hydroxymethyl-pyridin-3-yl)-pyridazin-3-yl]-1-methyl-ethyl}-amide as a brown solid.

1. additionwas added
2. customThe vial was flushed with argon
3. customsealed
4. additionThe reaction mixture was diluted with 2 mL of water
5. extractionextracted 4×4 mL with EtOAc
6. dry with materialThe combined organic layers were dried over MgSO4
7. filtrationfiltered
8. concentrationconcentrated
9. customPurification via normal phase flash chromatography on silica gel (0→4% MeOH/CH2Cl2)