Hydrochloric Acid → 6-Fluoropyridine-2-carbohydrazide

1,1-Dimethylethyl 2-[(6-fluoro-2-pyridinyl)carbonyl]hydrazinecarboxylate (510 mg, 2 mmol) was dissolved in 1,4-dioxane (5 mL) and treated with 4M HCl in 1,4 dioxane (5.00 mL, 20.00 mmol) at 0° C. The mixture was stirred to room temperature over 24 hr and was concentrated in vacuo, azeotroping with diethyl ether (3×50 ml) to afford a white solid. The solid was dissolved in methanol and loaded on to an SCX cartridge (Varian, 10 g), washing with methanol, and then eluting the product in free base form using 2M ammonia/methanol. The ammoniacal fractions were concentrated in vacuo to afford the product, 6-fluoro-2-pyridinecarbohydrazide (251 mg, 1.618 mmol).

1. concentrationwas concentrated in vacuo
2. customazeotroping with diethyl ether (3×50 ml)
3. customto afford a white solid
4. washwashing with methanol
5. washeluting the product in free base form
6. concentrationThe ammoniacal fractions were concentrated in vacuo

ORDレコード

ord-209a4ad2708244e2b62bc0630c3eb4b8

出典データセット

uspto-grants-2013_08

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08501946B2