反应详情

温度

90 °C

N-(7-Cyclopropylmethyl-4,5-dihydro-benzo[1,2-d;3,4-d′]bisthiazol-2-yl)-acetamide (Stage V.2, 180 mg, 0.589 mmol) was dissolved in EtOH (10 mL) and 36% HCl (1.193 g, 11.79 mmol) added. The RM was heated to 90° C. for 16 h then cooled and extracted with EtOAc/H2O. The organic layer was dried over Na2SO4 and evaporated. The crude material was chromatographed with MPLC C18 H2O 0.1% TFA/CH3CN 0.1% TFA, gradient 0-50%. Product containing fractions were neutralized with NaHCO3, extracted with EtOAc and lyophilized from dioxane to give the title compound (M+H=264.2; M−H=262.1; tR 4.183 min (Method F)).

1. temperaturethen cooled
2. extractionextracted with EtOAc/H2O
3. dry with materialThe organic layer was dried over Na2SO4
4. customevaporated
5. customThe crude material was chromatographed with MPLC
6. additionProduct containing fractions
7. extractionextracted with EtOAc