Ammonia → HCID 11770670, compound

HRID 1940258Notes

Reaction equation

HRID 1940258 reaction equation
Cl[P:2]1[C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=2[C:5]2[CH:12]=[CH:13][CH:14]=[CH:15][C:4]=2[O:3]1.[CH2:16]([OH:18])[CH3:17].N>C1(C)C=CC=CC=1>[CH2:16]([O:18][P:2]1[C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=2[C:5]2[CH:12]=[CH:13][CH:14]=[CH:15][C:4]=2[O:3]1)[CH3:17]

Participants

5

Reactant 3

HCID 222AmmoniaHCID 702EthanolHCID 898166H-Dibenz[c,e][1,2]oxaphosphorin, 6-chloro-

Product 1

HCID 11770670HCID 11770670, compoundYield 96%

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent2×

Procedure

300 g (1.28 mol) of 6-chloro-(6H)-dibenzo[c,e][1,2]-oxaphosphorine, dissolved in 346 ml of toluene, are added dropwise with stirring to a mixture of 76.5 g (1.663 mol) of absolute ethanol and 807 ml of toluene at -15° to -20° C. in the course of 1.5 hours. 23 g (1.35 mol) of ammonia are then introduced rapidly at this temperature. The mixture is further stirred and filtered off with suction and washed with toluene. The filtrate is concentrated by distillation at 12 mbar to an internal temperature of 75° C., finally at 1 mbar. 300 g of 6-ethoxy-(6H)-dibenzo[c,e][1,2]oxaphosphorine as solidified melt are obtained.

Workup

  1. additionare added dropwise
  2. filtrationfiltered off with suction
  3. washwashed with toluene
  4. concentrationThe filtrate is concentrated by distillation at 12 mbar to an internal temperature of 75° C., finally at 1 mbar

Sources & evidence

ORD record
ord-539238dd20484de6b32f6866ef880fc5
Source dataset
uspto-grants-1997_12
Patent number
US05698729

Reaction notes

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