Dimethylformamide → 4-Chloro-7-methoxyquinazolin-6-yl acetate--hydrogen chloride (1/1)

HRID 1793432ノート

反応式

HRID 1793432 の反応式
CN(C)C=O.[C:6]([O:9][C:10]1[CH:11]=[C:12]2[C:17](=[CH:18][C:19]=1[O:20][CH3:21])[N:16]=[CH:15][NH:14][C:13]2=O)(=[O:8])[CH3:7].S(Cl)([Cl:25])=O>>[ClH:25].[Cl:25][C:13]1[C:12]2[C:17](=[CH:18][C:19]([O:20][CH3:21])=[C:10]([O:9][C:6](=[O:8])[CH3:7])[CH:11]=2)[N:16]=[CH:15][N:14]=1

参加物

4

反応物 3

HCID 6228DimethylformamideHCID 24386Thionyl ChlorideHCID 1356819606-Acetoxy-7-methoxy-3H-quinazolin-4-one

生成物 1

HCID 220221594-Chloro-7-methoxyquinazolin-6-yl acetate--hydrogen chloride (1/1)収率 87%

実験手順

Dimethylformamide (0.25 ml) was added dropwise to a solution of 6-acetoxy-7-methoxy-3,4-dihydro-quinazolin-4-one (13.8 g, 59.0 mmol) in thionyl chloride (150 ml) and the reaction was heated at reflux for 1.5 hours. The reaction was cooled, excess thionyl chloride was removed in vacuo and the residue was azeotroped with toluene (2×50 ml) to remove the last of the thionyl chloride. Drying in vacuo yielded 4-chloro-6-acetoxy-7-methoxyquinazoline hydrochloride (14.7 g, 87% yield) as a beige solid, which was used without further purification:

後処理

  1. temperaturethe reaction was heated
  2. temperatureat reflux for 1.5 hours
  3. temperatureThe reaction was cooled
  4. customexcess thionyl chloride was removed in vacuo
  5. customthe residue was azeotroped with toluene (2×50 ml)
  6. customto remove the last of the thionyl chloride
  7. customDrying in vacuo

出典と根拠

ORDレコード
ord-1471d90fa01040128232ed4bb91f676d
出典データセット
uspto-grants-2006_07
特許番号
US07081461B1

反応ノート

読み込み中…