Cyanogen Bromide → HCID 13603543, compound

Temperature

0 °C

In a 250 ml round-bottom flask equipped with a mechanical stirrer were mixed (benzyloxythiocarbonyl)hydrazine and 2N sodium hydroxide (90 ml). This mixture was stirred vigorously and cooled to 0° C. A solution of cyanogen bromide (14.5 g, 0.137 mol) in methanol (60 ml) was added dropwise at a rate that kept the reaction temperature between about 0°-5° C. A precipitate formed. When the addition was complete, the reaction mixture was filtered and the residue was rinsed well with water and dried in vacuo. The product was recrystallized from methanol/water to give a white solid of 16.6 g, 58.5% yield with a m.p. of 173°-175° C.

1. customIn a 250 ml round-bottom flask equipped with a mechanical stirrer
2. custombetween about 0°-5° C
3. customA precipitate formed
4. additionWhen the addition
5. filtrationthe reaction mixture was filtered
6. washthe residue was rinsed well with water
7. customdried in vacuo
8. customThe product was recrystallized from methanol/water
9. customto give a white solid of 16.6 g, 58.5% yield with a m.p. of 173°-175° C.

ORD record

ord-651800e9c125450ebd980fea39e0a11e

Source dataset

uspto-grants-1986_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04576629