Hydrochloric Acid → 1,2-Thiazole-5-carbohydrazide

A mixture of 1,1-dimethylethyl 2-(5-isothiazolylcarbonyl)hydrazinecarboxylate (I83) (480 mg, 1.973 mmol) in HCl (2 ml, 8.00 mmol) (4M in 1,4-dioxan) was stirred at room temperature under argon for 18 hours (overnight). After this time, the mixture was concentrated under reduced pressure to give a pale yellow coloured solid. The solid was dissolved in MeOH and passed through and SCX cartridge, eluting initially with MeOH and then with 2M NH3 in MeOH. The NH3/MeOH fractions were concentrated under reduced pressure to give a yellow coloured solid in 217 mg.

1. concentrationAfter this time, the mixture was concentrated under reduced pressure
2. customto give a pale yellow coloured solid
3. washeluting initially with MeOH
4. concentrationThe NH3/MeOH fractions were concentrated under reduced pressure
5. customto give a yellow coloured solid in 217 mg

ORD-Eintrag

ord-f2529446cf7d489fa598a871347a2e86

Quelldatensatz

uspto-grants-2013_08

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08501946B2