反应详情

1-Chloroethyl chloroformate (0.034 mL, 0.31 mmol) was added to a stirred solution of 5,6,7,8-tetrahydro-2-(phenoxymethyl)-5-(phenylmethyl)-4H-thiazolo[5,4-c]azepine (0.055 mg, 0.16 mmol) and DIPEA (0.08 mL, 0.47 mmol) in DCM (1 mL). The mixture was stirred at room temperature for 1 hour. Then, the solvent was evaporated in vacuo and a solution of the crude product in MeOH (1 mL) was stirred at 70° C. for 1 hour. The mixture was treated with a 7M solution of ammonia in MeOH and the solvents evaporated in vacuo. The crude product was purified by flash column chromatography (silica; 7 M solution of ammonia in MeOH in DCM 0/100 to 3 /97). The desired fractions were collected and the solvents evaporated in vacuo to yield 5,6,7,8-tetrahydro-2-(phenoxymethyl)-4H-thiazolo[5,4-c]azepine (0.033 g, 81% yield) as a yellow oil. C14H16N2OS LCMS: Rt 1.13, m/z 302 [M+ACN+H]+ (using method, LC-MS Method 6).

1. customThen, the solvent was evaporated in vacuo
2. stirringa solution of the crude product in MeOH (1 mL) was stirred at 70° C. for 1 hour
3. additionThe mixture was treated with a 7M solution of ammonia in MeOH
4. customthe solvents evaporated in vacuo
5. customThe crude product was purified by flash column chromatography (silica; 7 M solution of ammonia in MeOH in DCM 0/100 to 3 /97)
6. customThe desired fractions were collected
7. customthe solvents evaporated in vacuo