Diethylamine → 1636-15-3

HRID 748598Notes

Reaction equation

HRID 748598 reaction equation
[C:1]1([P:7]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)Cl)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH2:15]([NH:17][CH2:18][CH3:19])[CH3:16]>C1(C)C=CC=CC=1>[P:7]([N:17]([CH2:18][CH3:19])[CH2:15][CH3:16])([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)[C:1]1[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

Participants

4

Reactant 2

HCID 8021DiethylamineHCID 66180Chlorodiphenylphosphine

Product 1

HCID 121407181636-15-3

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent

Procedure

Diphenylchlorophosphine (2.0 mL, 2.38 g, 10.79 mmol) was added to a stirred solution of diethylamine (2.5 mL, 1.82 g, 24.9 mmol) in toluene (20 mL). The resulting white slurry was stirred overnight at ambient temperature and filtered. The filtered solid was washed with toluene (2×10 mL). The combined filtrate was reduced in volume by distillation in vacuum to approximately 20 mL and transferred to a graduated Schlenk tube equipped with a Yong valve. The volume of the solution was adjusted to 31.0 mL by addition of toluene to give 0.348 M solution of Ph2PNEt2. 31P{1H} NMR (toluene, 25° C.), δ: 51.0 (s).

Workup

  1. filtrationfiltered
  2. washThe filtered solid was washed with toluene (2×10 mL)
  3. distillationThe combined filtrate was reduced in volume by distillation in vacuum to approximately 20 mL
  4. customtransferred to a graduated Schlenk tube
  5. customequipped with a Yong valve
  6. additionThe volume of the solution was adjusted to 31.0 mL by addition of toluene

Sources & evidence

ORD record
ord-a36931dd06a24e8c920955b10b7087e3
Source dataset
uspto-grants-2008_07
Patent number
US07399859B1

Reaction notes

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