Hydroxylamine → HCID 76979141, compound

Temperature

90 °C

To a suspension of tetrahydro-pyran-4-carbaldehyde (36.9 g, 259 mmol) and hydroxylamine (27.2 g, 388 mmol) in ethanol (246 mL) and water (246 mL) was added sodium acetate) 42.9 g, 517 mmol) and the resulting mixture heated at 90° C. overnight. After cooling to room temperature the resulting mixture was then evaporated and extracted with diethylether and water. The organic extract was then washed with water, brine, dried over sodium sulfate and evaporated. Purification by chromatography (silica, heptane:ethyl acetate=1:1) afforded the title compound (16.8 g, 50%) which was obtained as a yellow liquid. MS: m/e=129.1 [M+H]+.

1. temperatureAfter cooling to room temperature the resulting mixture
2. customwas then evaporated
3. extractionextracted with diethylether and water
4. extractionThe organic extract
5. washwas then washed with water, brine
6. dry with materialdried over sodium sulfate
7. customevaporated
8. customPurification by chromatography (silica, heptane:ethyl acetate=1:1)

ORD record

ord-fb571e45c36c40b28930762d6d504ac1

Source dataset

uspto-grants-2013_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08357703B2