反应详情

The title compound of example 31.1 (1.0 g, 5.98 mmol) was stirred in methanol (6 mL) at 60° C. Methyl isothiocyanate (481 mg, 6.58 mmol) was dissolved in methanol (2 mL) and added to the reaction mixture which was stirred for 15 min. After 15 min a solution of sodium hydroxide (263 mg) in water (2 mL) was added to the reaction mixture which was kept stirring at 60° C. overnight. The reaction mixture was then concentrated in vacuo to remove the methanol and the remaining residue was stirred in 3 M HCl (aq) to precipitate the product which was collected by vacuum filtration (off-white powder, 1.2 g, 90%).

1. additionadded to the reaction mixture which
2. stirringwas kept stirring at 60° C. overnight
3. concentrationThe reaction mixture was then concentrated in vacuo
4. customto remove the methanol
5. stirringthe remaining residue was stirred in 3 M HCl (aq)
6. customto precipitate the product which
7. filtrationwas collected by vacuum filtration (off-white powder, 1.2 g, 90%)