1,3-Propanediol → HCID 18673603, compound

Temperature

0 °C

3.7 g(49 mmol) of 1,3-propandiol was dissolved in 50 ml of dimethylformamide and cooled to 0° C. 2 g(50 mmol) of 60% sodium hydride dispersed in mineral oil was added slowly. After the mixture was stirred for 10 minutes, 10 g(49 mmol) of 2-chlorobenzyl-bromide dissolved in 10 ml of dimethyformamide was added slowly. After stirring for one hour at room temperature, dimethylformamide was removed under reduced pressure, 100 ml of ethylacetate was added to the residue and the organic layer was washed with saturated sodium chloride solution (100 ml×3). The organic layer was dried over anhydrous magnesium sulfate and concentrated. The residue was subjected to column chromatography(eluent: n-hexane/ethylacetate=4/1, v/v) to give 3.52 g(Yield 35.8%) of the title compound.

1. additionwas added slowly
2. additionwas added slowly
3. stirringAfter stirring for one hour at room temperature
4. customdimethylformamide was removed under reduced pressure, 100 ml of ethylacetate
5. additionwas added to the residue
6. washthe organic layer was washed with saturated sodium chloride solution (100 ml×3)
7. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
8. concentrationconcentrated

ORD record

ord-5adbafcb454c4138b734bc549fd018ff

Source dataset

uspto-grants-2003_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06511978B1