Triethylamine → HCID 131721614, compound

HRID 850686Notes

Reaction equation

HRID 850686 reaction equation
[P:1]([NH:11][CH2:12][CH3:13])([NH:8][CH2:9][CH3:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[P:14](Cl)([C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1)[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1.CCN([CH2:33][CH3:34])CC>C(Cl)Cl>[P:14]([N:11]([P:1]([N:8]([P:14]([C:34]1[CH:33]=[CH:26][CH:21]=[CH:22][CH:23]=1)[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)[CH2:9][CH3:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1)[CH2:12][CH3:13])([C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1)[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1

Participants

5

Reactant 3

HCID 8471TriethylamineHCID 66180ChlorodiphenylphosphineHCID 12782703N,N′-Diethyl-P-phenylphosphonous diamide

Product 1

HCID 131721614HCID 131721614, compoundYield 86.7%

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

A solution of PPh(NHEt)2 (0.301 g, 1.5 mmol) in CH2CH2 (20 cm3) was added to PPh2Cl (0.677 g, 3.0 mmol) dissolved in CH2Cl2 (5 cm3) containing NEt3 (0.466 g, 4.6 mmol) and stirred for two hours. The solvent was removed in vacuo affording an off white solid. The solid was washed with 3×20 cm3 aliquots of diethylether, the washings combined and the solvent then removed in vacuo yielding a white solid characterised as Ph2PN(Et)P(Ph)N(Et)PPh2 (0.54 g 1.3 mmol) 31P [H] NMR (CD2Cl2)=53.5 [d, PPh2, 2P, J (PP) 25]. 105.1 [t, PPh, J(PP) 25 Hz] ppm.

Workup

  1. customThe solvent was removed in vacuo
  2. customaffording an off white solid
  3. washThe solid was washed with 3×20 cm3 aliquots of diethylether
  4. customthe solvent then removed in vacuo

Sources & evidence

ORD record
ord-73eac2533eb044788d87c32364ea1c00
Source dataset
uspto-grants-2000_01
Patent number
US06018016

Reaction notes

Loading…