1-Dodecanol → HCID 15375359, compound
Reaction equation
[CH2:1](O)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12].[P:14]([Cl:18])(Cl)(Cl)=[O:15]>C(Cl)Cl>[CH2:1]([P:14]([Cl:18])([CH2:12][CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2][CH3:1])=[O:15])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12]Participants
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
223.6 Grams (1.2 mol) of dodecyl alcohol and 500 ml of methylene chloride were placed in 1-liter three-necked flask equipped with a condenser and a stirrer; then 55.8 g (0.6 mol) of phosphorus oxychloride was added dropwise over 30 min, with stirring, under cooling with ice with the internal temperature kept below 10° C.; and after the completion of the addition the stirring was continued for 20 min. The temperature of this reaction mixture was elevated to room temperature, then the reaction was continued for 1 hour under reduced pressure of 80 to 120 mmHg; and after the temperature was elevated to 50° C., the reaction was continued for 3 hours under ordinary pressures. The reaction mixture was cooled to room temperature, to obtain 246.6 g (yield: 87.6%) of a transparent liquid.
Workup
- customequipped with a condenser and a stirrer
- temperatureunder cooling with ice with the internal temperature
- customkept below 10° C.
- additionand after the completion of the addition the stirring
- customwas elevated to room temperature
- waitthe reaction was continued for 1 hour under reduced pressure of 80 to 120 mmHg
- customwas elevated to 50° C.
- waitthe reaction was continued for 3 hours under ordinary pressures
Sources & evidence
- ORD record
- ord-d08addd295264ee8be27fb54d52348c1
- Source dataset
- uspto-grants-1996_08
- Patent number
- US05543288
Reaction notes
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