Methanol → HCID 21183889, compound

HRID 1938543Notes

Reaction equation

HRID 1938543 reaction equation
[Cl:1][C:2]1[N:11]=[C:10](Cl)[C:9]2[C:4](=[C:5]([O:17][CH3:18])[C:6]([O:15][CH3:16])=[C:7]([O:13][CH3:14])[CH:8]=2)[N:3]=1.[H-].[Na+].[CH3:21][OH:22]>>[Cl:1][C:2]1[N:11]=[C:10]([O:22][CH3:21])[C:9]2[C:4](=[C:5]([O:17][CH3:18])[C:6]([O:15][CH3:16])=[C:7]([O:13][CH3:14])[CH:8]=2)[N:3]=1

Participants

4

Reactant 3

HCID 887MethanolHCID 24758Sodium hydrideHCID 12320025HCID 12320025, compound

Product 1

HCID 21183889HCID 21183889, compoundYield 97%

Procedure

5.00 g (17.3 mmol) of 2,4-dichloro-6,7,8-trimethoxyquinazoline was suspended in 100 ml of methanol, followed by the gradual addition of 1.5 g of sodium hydride. The obtained mixture was heated under reflux. After several hours, the reaction mixture was concentrated under a reduced pressure, followed by the addition of water. The crystal thus precipitated was recovered by filtration, washed with water and air-dried to give 4.80 g of the title compound as a pale-pink crystal.

Workup

  1. temperatureThe obtained mixture was heated
  2. temperatureunder reflux
  3. waitAfter several hours
  4. concentrationthe reaction mixture was concentrated under a reduced pressure
  5. additionfollowed by the addition of water
  6. customThe crystal thus precipitated
  7. filtrationwas recovered by filtration
  8. washwashed with water
  9. customair-dried

Sources & evidence

ORD record
ord-9644c33c41be488bb3b90ab038431fc9
Source dataset
uspto-grants-1997_12
Patent number
US05693652

Reaction notes

Loading…