Reaction equation
C(Cl)(=[O:3])C.[P:5]([O:14][CH2:15][CH2:16][Cl:17])([O:10][CH2:11][CH2:12][Cl:13])[O:6][CH2:7][CH2:8]Cl>C(Cl)CCl>[P:5]([O:14][CH2:15][CH2:16][Cl:17])([O:10][CH2:11][CH2:12][Cl:13])[O:6][C:7](=[O:3])[CH3:8]Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
The same equipment and procedure as in Example 1 was employed. The reaction flask was charged with 100 ml ethylene dichloride and 85 g acetyl chloride (1.1 mole). The addition of 270 g (1.0 mole) tris (β-chloroethyl) phosphite was commenced dropwise and continued for one hour during which there was a slow exotherm to 35° C. After addition of the triphosphite the reaction continued with a self-maintained exotherm at about 40° C. for three hours and then a slow return to ambient temperature while stirring overnight. The pink acetyl bis(β-chloroethyl) phosphite was isolated by rotary evaporatory at 50° C. and 15 torr. The yield was 261 g; acid number 2; purity by infrared analysis was about 75%.
Workup
- customto 35° C
- waitcontinued with a self-maintained exotherm at about 40° C. for three hours
Sources & evidence
- ORD record
- ord-7f2eae64cf9d43a7a79072298464b4a8
- Source dataset
- uspto-grants-1983_10
- Patent number
- US04407765
Linked notes
Loading…