反应详情

温度

50 °C

In a 5 mL microwave vial, (Z)-methyl N′-cyano-N-(3,5-dichlorophenyl)carbamimidothioate (156 mg, 0.6 mmol, Eq: 1.00), hydroxylamine hydrochloride (347 mg, 5 mmol, Eq: 8.33) and triethylamine (506 mg, 697 μl, 5 mmol, Eq: 8.33) were combined with DMF (6 ml) to give a white suspension. The vial capped and stirred in a 50° C. oil bath for 3.5 hours. The reaction was concentrated in vacuo and the crude material was purified by preparative TLC (silica gel, 1.0 mm, 9:1 DCM/MeOH) to give product, was recrystallized from EtOH then dried in vacuo (80° C., 2 torr, overnight) to give 15 mg (10%) of desired product as a white solid.

1. customto give a white suspension
2. customThe vial capped
3. concentrationThe reaction was concentrated in vacuo
4. customthe crude material was purified by preparative TLC (silica gel, 1.0 mm, 9:1 DCM/MeOH)
5. customto give product
6. customwas recrystallized from EtOH
7. customthen dried in vacuo (80° C., 2 torr, overnight)