Phosphorus oxychloride → HCID 117772417, compound

HRID 2281109Notes

Reaction equation

HRID 2281109 reaction equation
[Cl:1][C:2]1[CH:11]=[C:10]([I:12])[CH:9]=[C:8]2[C:3]=1[C:4](=O)[NH:5][CH:6]=[N:7]2.CCN(C(C)C)C(C)C.O=P(Cl)(Cl)[Cl:25]>C1(C)C=CC=CC=1>[Cl:25][C:4]1[C:3]2[C:8](=[CH:9][C:10]([I:12])=[CH:11][C:2]=2[Cl:1])[N:7]=[CH:6][N:5]=1

Participants

5

Reactant 3

HCID 24813Phosphorus oxychlorideHCID 81531DiisopropylethylamineHCID 136927191HCID 136927191, compound

Product 1

HCID 117772417HCID 117772417, compound

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent

Procedure

To a mixture of 0.4 g (1.27 mmol) 5-chloro-7-iodo-3H-quinazolin-4-one, 0.5 ml (3.18 mmol) DIPEA and toluene, 0.3 ml (2.8 mmol) POCl3 is added dropwise and stirred at RT for 1 h, the heated to 90° C. for 1.5 h. After cooling to RT the solvent is evaporated giving rise to crude 4,5-dichloro-7-iodo-quinazoline.

Workup

  1. additionis added dropwise
  2. temperaturethe heated to 90° C. for 1.5 h
  3. temperatureAfter cooling to RT the solvent
  4. customis evaporated

Sources & evidence

ORD record
ord-1b6236effec14b4caec9030ee3e4c806
Source dataset
uspto-grants-2015_09
Patent number
US09139577B2

Reaction notes

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