Triethylamine → HCID 86609193, compound

HRID 1180661Notes

Reaction equation

HRID 1180661 reaction equation
[P:1]([Cl:5])(Cl)([Cl:3])=[O:2].[CH3:6][CH:7]([CH:13]([CH2:16][CH2:17][CH:18]([CH3:24])[CH2:19][C:20]([CH3:23])([CH3:22])[CH3:21])[CH2:14][OH:15])[CH2:8][C:9]([CH3:12])([CH3:11])[CH3:10].C(N(CC)CC)C>C1(C)C=CC=CC=1>[CH3:6][CH:7]([CH:13]([CH2:16][CH2:17][CH:18]([CH3:24])[CH2:19][C:20]([CH3:21])([CH3:23])[CH3:22])[CH2:14][O:15][P:1]([Cl:5])([Cl:3])=[O:2])[CH2:8][C:9]([CH3:10])([CH3:11])[CH3:12]

Participants

5

Reactant 3

HCID 8471TriethylamineHCID 24813Phosphorus oxychlorideHCID 2563715,7,7-Trimethyl-2-(1,3,3-trimethylbutyl)-1-octanol

Product 1

HCID 86609193HCID 86609193, compoundYield 34.7%

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent

Conditions

Temperature
-10 °C

Procedure

With nitrogen substitution, 540 ml of toluene and 138.0 grams (0.9 moles) of phosphorus oxychloride were added and cooled to −10 degrees C. To this mixture, a solution of 243.5 grams (0.9 moles; 1.0 in molar ratio) of 2-(1,3,3-trimethyl-n-butyl)-5,7,7-trimethyl-n-octanol and 91.1 grams (0.9 moles) of triethylamine was dripped, and the mixture was reacted for 12 hours at 0 degrees C. The mixture was then heated to 25 degrees C., and a triethylamine hydrochloride was removed by filtering to obtain 1003.9 grams of a toluene solution of [2-(1,3,3-trimethyl-n-butyl)-5,7,7-trimethyl-n-octyl]dichlorophosphate (34.7% in concentration).

Workup

  1. customthe mixture was reacted for 12 hours at 0 degrees C
  2. temperatureThe mixture was then heated to 25 degrees C
  3. custom, and a triethylamine hydrochloride was removed
  4. filtrationby filtering

Sources & evidence

ORD record
ord-d2c382dfe7ed4c98990632e31a973def
Source dataset
uspto-grants-2007_10
Patent number
US07282597B2

Reaction notes

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