Imidazole → 1,1,1-Trifluoro-4-iodo-2-butanol

A solution of triphenylphosphine (1.09 g, 4.16 mmol) in dichloromethane (14 mL) was treated with imidazole (0.283 g, 4.16 mmol) and iodine (1.06 g, 4.16 mmol), respectively, to give an orange suspension. A solution of 4,4,4-trifluoro-1,3-butanediol (0.500 g, 3.47 mmol) in dichloromethane (4 mL) was added to the suspension and stirred for 20 minutes. The solid was removed by filtration and the filtrate was concentrated under reduced pressure without heat to yield a black oil. The crude oil was purified by silica gel chromatography, eluting with 100% dichloromethane, to give the product as an oil (0.640 g, 72%).

1. customrespectively, to give an orange suspension
2. customThe solid was removed by filtration
3. concentrationthe filtrate was concentrated under reduced pressure
4. temperaturewithout heat
5. customto yield a black oil
6. customThe crude oil was purified by silica gel chromatography
7. washeluting with 100% dichloromethane

ORDレコード

ord-b709147a52554af893f0701a50fc4f75

出典データセット

uspto-grants-2006_10

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07119109B2