Phosphorus oxychloride → HCID 85817173, compound

HRID 2211977Notes

Reaction equation

HRID 2211977 reaction equation
O=[C:2]([CH3:18])[CH:3]([NH:9][C:10]([C:12]1[CH:13]=[N:14][CH:15]=[CH:16][CH:17]=1)=[O:11])[CH2:4][C:5]([O:7][CH3:8])=[O:6].P(Cl)(Cl)(Cl)=O>C1(C)C=CC=CC=1>[CH3:18][C:2]1[O:11][C:10]([C:12]2[CH:13]=[N:14][CH:15]=[CH:16][CH:17]=2)=[N:9][C:3]=1[CH2:4][C:5]([O:7][CH3:8])=[O:6]

Participants

4

Reactant 2

HCID 24813Phosphorus oxychlorideHCID 21962868HCID 21962868, compound

Product 1

HCID 85817173HCID 85817173, compoundYield 108.7%

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent

Procedure

Intermediate 32 (110 mg) was treated with phosphorous oxychloride (0.51 ml) in toluene (2 ml) and the mixture heated under reflux for 3.5 h. The mixture was poured into ice cold saturated aqueous sodium bicarbonate (30 ml) and extracted with dichloromethane (20 ml). The organic layer was evaporated in vacuo to give a yellow gum (111 mg).

Workup

  1. temperaturethe mixture heated
  2. temperatureunder reflux for 3.5 h
  3. extractionextracted with dichloromethane (20 ml)
  4. customThe organic layer was evaporated in vacuo

Sources & evidence

ORD record
ord-a45d0f1d4b034071b7516b4347ebde08
Source dataset
uspto-grants-2006_09
Patent number
US07101882B2

Reaction notes

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