Benzylamine → AC1MDMFL

HRID 1780217Notes

Reaction equation

HRID 1780217 reaction equation
[Cl:1][CH2:2][P:3]([CH2:6]Cl)(=[O:5])[OH:4].[CH2:8]([NH2:15])[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1>>[ClH:1].[CH2:8]([NH:15][CH2:2][P:3]([CH2:6][NH:15][CH2:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)(=[O:5])[OH:4])[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1

Participants

3

Reactant 2

HCID 7504BenzylamineHCID 574694Bis(chloromethyl)phosphinic acid

Product 1

HCID 2839277AC1MDMFL

Conditions

Temperature
115 °C

Procedure

12 g (74 mmol) of bis(chloromethyl)phosphinic acid are added slowly to 80 g of benzylamine at room temperature while stirring, during which the temperature increases slightly. The mixture is then heated at 115° C. for 24 h. Excess benzylamine is removed by distillation in vacuo, and the white residue is dissolved in 150 ml of distilled water, filtered and mixed with 30 mi of concentrated HCl and stirred at room temperature for 1 h. The white precipitate is filtered off with suction, washed with water and dried over P2O5. Yield: 20 g (79%); m.p.: 254° C.

Workup

  1. temperatureincreases slightly
  2. customExcess benzylamine is removed by distillation in vacuo
  3. dissolutionthe white residue is dissolved in 150 ml of distilled water
  4. filtrationfiltered
  5. additionmixed with 30 mi of concentrated HCl
  6. stirringstirred at room temperature for 1 h
  7. filtrationThe white precipitate is filtered off with suction
  8. washwashed with water
  9. dry with materialdried over P2O5

Sources & evidence

ORD record
ord-7413cd76a3d14d178dc63224d0fe8ee5
Source dataset
uspto-grants-1997_05
Patent number
US05629431

Reaction notes

Loading…