Sodium Hydroxide → 3-Bromo-thiophene-2-carbaldehyde oxime

Temperature

0 °C

3-Bromothiophene-2-carbaldehyde (maybridge) (28.7 gm, 0.15 mol) in ethanol (50 ml) was added in one portion to a solution of hydroxylamine hydrochloride (13.8 gm, 0.2 mole), sodium hydroxide (8 gm, 0.2 mol) in water (30 ml) and ethanol (100 ml). The mixture was stirred at 0° C. for 2 hours and was kept at 0° C. overnight. The reaction mixture was diluted with cold water (600 ml), and the precipitated solids were collected by filtration to provide 20.5 gm, (67%) of product. The aqueous layer was further extracted with ethyl acetate and, the combined organic layers were washed with brine, dried with magnesium sulfate filtered and concentrated in vacuo to leave an additional 6.9 g of product.

1. waitwas kept at 0° C. overnight
2. filtrationthe precipitated solids were collected by filtration

ORD record

ord-719ea8f2e9e04de8b90d6cc4d0bd502f

Source dataset

uspto-grants-2009_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07550469B2