Dicyclohexylamine → 6-(N,N-Di-cyclohexyl-amino)-dibenz[c,e][1,2]oxaphosphorine

HRID 1702130Notes

Reaction equation

HRID 1702130 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.[CH:16]1([NH:22][CH:23]2[CH2:28][CH2:27][CH2:26][CH2:25][CH2:24]2)[CH2:21][CH2:20][CH2:19][CH2:18][CH2:17]1.C(N(CC)CC)C>C1(C)C=CC=CC=1>[CH:23]1([N:22]([P:2]2[C:7]3[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=3[C:5]3[CH:12]=[CH:13][CH:14]=[CH:15][C:4]=3[O:3]2)[CH:16]2[CH2:17][CH2:18][CH2:19][CH2:20][CH2:21]2)[CH2:24][CH2:25][CH2:26][CH2:27][CH2:28]1

Participants

5

Reactant 3

HCID 7582DicyclohexylamineHCID 8471TriethylamineHCID 898166H-Dibenz[c,e][1,2]oxaphosphorin, 6-chloro-

Product 1

HCID 205041466-(N,N-Di-cyclohexyl-amino)-dibenz[c,e][1,2]oxaphosphorine

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent

Procedure

35.1 g (0.15 mol) of 6-chloro-dibenz[c,e][1,2]oxaphosphorine, 27.1 g (0.15 mol) of dicyclohexylamine and 50 ml of triethylamine are kept at reflux temperature for 10 hours. Toluene is added to the solution; the triethylamine hydrochloride is then removed by filtration, and the filtrate is concentrated in vacuo. The crystalline product has a melting point of 162° C. (Compound I).

Workup

  1. temperatureat reflux temperature for 10 hours
  2. customthe triethylamine hydrochloride is then removed by filtration
  3. concentrationthe filtrate is concentrated in vacuo

Sources & evidence

ORD record
ord-8997c1d832b343b2a7cb877c766f8f66
Source dataset
uspto-grants-1983_04
Patent number
US04380515

Reaction notes

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