Ammonia → Methoxydiphenylphosphine

HRID 1421656Notes

Reaction equation

HRID 1421656 reaction equation
[CH2:1]([OH:3])C.Cl[P:5]([C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1.N>>[C:12]1([P:5]([C:6]2[CH:7]=[CH:8][CH:9]=[CH:10][CH:11]=2)[O:3][CH3:1])[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=1

Participants

4

Reactant 3

HCID 222AmmoniaHCID 702EthanolHCID 66180Chlorodiphenylphosphine

Product 1

HCID 77636MethoxydiphenylphosphineYield 73%

Procedure

210 g (6.56 mol) of absolute ethanol are cooled to -15° C. under a nitrogen atmosphere. 200 g (0.907 mol) of chloro(diphenyl)phosphine are then added dropwise at this temperature with vigorous stirring. 18 g (1.06 mol) of ammonia gas are then introduced. The mixture is then stirred without cooling for 10 hours and filtered by suction. The filtrate is freed from methanol and excess ammonia in vacuo. The residue is filtered by suction through a glass frit. 143 g of crude methyl diphenylphosphinite are obtained. This corresponds to a yield of 73% of theory.

Workup

  1. temperaturewithout cooling for 10 hours
  2. filtrationfiltered by suction
  3. filtrationThe residue is filtered by suction through a glass frit

Sources & evidence

ORD record
ord-b2e9208d77df424987813b0a7f5486e7
Source dataset
uspto-grants-2000_06
Patent number
US06077968

Reaction notes

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