Hydrochloric Acid → HCID 71224690, compound

2 mL of a chloroform solution containing 0.24 g (1 mmol) of 2-t-butoxycarbonyl amino-6-methylpyridine and 0.26 g (2 mmol) of diisopropylethylamine was prepared, and was cooled in ice water. The above mixed solution was added dropwise at 0° C. to 0.3 mL of a chloroform solution containing 0.11 g (1.2 mmol) of methyl chloroformate. After stirring further for 20 minutes, the temperature was raised to room temperature. After stirring further for 5 hours at room temperature, 5 mL of water and 1 mL of 3N hydrochloric acid were added thereto, followed by liquid separation. The organic layer obtained by liquid separation was dried with magnesium sulfate, followed by filtration, and the resulting solution was concentrated under reduced pressure to obtain 0.27 g of 2-t-butoxycarbonyl-methoxycarbonyl amino-6-methyl pyridine-N-oxide (yield: 96%) as a pale yellow oily liquid which was the target product.

1. customwas prepared
2. additionThe above mixed solution
3. stirringAfter stirring further for 5 hours at room temperature
4. customfollowed by liquid separation
5. customThe organic layer obtained by liquid separation
6. dry with materialwas dried with magnesium sulfate
7. filtrationfollowed by filtration
8. concentrationthe resulting solution was concentrated under reduced pressure

ORD record

ord-b9d96af0a4fb4541b82f3fbbbbb8af4c

Source dataset

uspto-grants-2015_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08981107B2