Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | 1-Dodecanol | HCID 8193 | — |
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 15375359 | HCID 15375359 | 97.6% |
Reaction Steps
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.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US05543288 |
|---|
| Source dataset | uspto-grants-1996_08 |
|---|
| ORD ID | ord-d08addd295264ee8be27fb54d52348c1 |
|---|
| Source note | uspto-grants-1996_08 |
|---|