Methyl isobutyrate → HCID 16062603, compound

Temperature

-78 °C

A 2.86 g quantity (28 mmole) of methyl isobutyrate was dissolved in 25 ml of THF, and the mixture was chilled to −78° C. under argon atmosphere. To the mixture was slowly added dropwise 14.0 ml (28 mmole) of lithium diisopropylamide (Aldrich Corp., 2.0M heptane.THF.ethylbenzene solution) over a period of 10 minutes. The reaction mixture was gradually heated (one hour) and thereto was added dropwise a solution of 8.9 g of dimethylbismuthanyl bromide prepared in Preparation Example 2 in 25 ml of THF between −40° C. and −30° C. The reaction mixture was further stirred until reached to 0° C. (one hour). After the solids were filtrated with quartz wool and THF was removed in a vacuum, the reaction mixture was distilled in a vacuum, giving 4.45 g (yield 46.7%) of a yellow oily product. b.p. 59° C./2.0 mmHg.

1. temperatureThe reaction mixture was gradually heated (one hour)
2. customuntil reached to 0° C.
3. custom(one hour)
4. filtrationAfter the solids were filtrated with quartz wool and THF
5. customwas removed in a vacuum
6. distillationthe reaction mixture was distilled in a vacuum

ORD record

ord-739177a449494a5894dbc53345ed4a0b

Source dataset

uspto-grants-2010_12

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07847043B2