Diisopropylamine → HCID 23278438, compound

HRID 1190793Notes

Reaction equation

HRID 1190793 reaction equation
[CH:1]([NH:4][CH:5]([CH3:7])[CH3:6])([CH3:3])[CH3:2].[C:8]1([P:14](Cl)[Cl:15])[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1>CCCCCC>[Cl:15][P:14]([N:4]([CH:5]([CH3:7])[CH3:6])[CH:1]([CH3:3])[CH3:2])[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1

Participants

4

Reactant 2

HCID 7912DiisopropylamineHCID 12573Phenyl phosphorus dichloride

Product 1

HCID 23278438HCID 23278438, compoundYield 80%

Reagents, catalysts & solvents 1

HCID 8058HexaneSolvent2×

Conditions

Temperature
0 °C

Procedure

A solution of diisopropylamine (8.90 grams, 88.3 mmol) in dry hexane (100 ml) was added dropwise to a stirred solution of phenyldichlorophosphine (7.91 grams, 44.2 mmol) in hexane (100 ml) cooled to 0° C., during 45 minutes. The resulting mixture was allowed to warm to room temperature and was then stirred for additional 18 hours and thereafter filtered. The precipitate was washed with hexane, and the product was further purified by distillation under reduced pressure, to give 8.62 grams (80% yield) of Compound 59 (see, Scheme 34 below) as a colorless oil.

Workup

  1. temperatureto warm to room temperature
  2. filtrationfiltered
  3. washThe precipitate was washed with hexane
  4. distillationthe product was further purified by distillation under reduced pressure

Sources & evidence

ORD record
ord-267bed69eea14c52b8296a12482ef278
Source dataset
uspto-grants-2014_03
Patent number
US08680062B2

Reaction notes

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