Imidazole → (R)-1-iodo-2,6-dimethyl heptane

To a mixture of supported triphenyl phosphine (6.55 g, 19.67 mmol) in CH2Cl2 at 0° C. was added iodine (4.99 g, 19.67 mmol) and imidazole (1.33 g, 19.67 mmol). The mixture was warmed to ambient temperature, stirred for 1 h and cooled to 0° C. for the dropwise addition of (R)-2,6-dimethyl heptan-1-ol in CH2Cl2 (5 mL). The mixture was allowed to reach ambient temperature and stirred for 1 h, at which time it was filtered through a pad of celite and the solids were washed with CH2Cl2. The filtrated was concentrated, and the crude product was purified via silica gel chromatography to give (R)-1-iodo-2,6-dimethyl heptane (2.44 g).

1. customto reach ambient temperature
2. stirringstirred for 1 h, at which time it
3. filtrationwas filtered through a pad of celite
4. washthe solids were washed with CH2Cl2
5. concentrationThe filtrated was concentrated
6. customthe crude product was purified via silica gel chromatography

ORDレコード

ord-79cb949d838e4477b5d7a1551591ef04

出典データセット

uspto-grants-2008_09

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07419981B2