Chloroform → HCID 20493128, compound

To a solution of 17.2 g of dimethyl vinyl carbinol in 150 ml of chloroform was added 0.8 g of benzoyl peroxide and, in an autoclave, the mixture was reacted at 135° C. and in a nitrogen atmosphere for 18 hours. Then, the unreacted dimethyl vinyl carbinol and chloroform were removed by distillation under reduced pressure. As the residue was obtained 30.1 g of a dark-reddish viscous fluid. This residue was subjected to vacuum distillation to obtain 28.2 g (yield 69%) of 1,1,1-trichloro-4-pentanol. Gas-chromatographic analysis of this product showed its purity to be 95.4%. mass spectrometric data suggested that the impurity comprised 1,1,3-trichloro-4-methyl-4-pentanol. The following procedures were used for structural identification of 1,1,1-trichloro-4-methyl-4-pentanol.

1. customin an autoclave, the mixture was reacted at 135° C. and in a nitrogen atmosphere for 18 hours
2. customThen, the unreacted dimethyl vinyl carbinol and chloroform were removed by distillation under reduced pressure
3. customAs the residue was obtained 30.1 g of a dark-reddish viscous fluid
4. distillationThis residue was subjected to vacuum distillation

ORD record

ord-259f2d60c509449db3f64e388e817f21

Source dataset

uspto-grants-1983_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

USRE031330