Phosphorus oxychloride → 7-Bromo-4-chloro-2-methoxyquinazoline

HRID 1473664ノート

反応式

HRID 1473664 の反応式
[Br:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6](=O)[NH:7][C:8]([O:12][CH3:13])=[N:9]2)=[CH:4][CH:3]=1.C1CCN2C(=NCCC2)CC1.O=P(Cl)(Cl)[Cl:28]>C(Cl)Cl>[Br:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6]([Cl:28])=[N:7][C:8]([O:12][CH3:13])=[N:9]2)=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 24813Phosphorus oxychlorideHCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 1364090737-bromo-2-methoxyquinazolin-4(3H)-one

生成物 1

HCID 866877407-Bromo-4-chloro-2-methoxyquinazoline

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A solution of 7-bromo-2-methoxyquinazolin-4(3H)-one (1.900 g, 7.45 mmol) in 30 mL DCM was treated with DBU (1.123 ml, 7.45 mmol) and was allowed to stir for 20 minutes. The cloudy purple solution was then treated with POCl3 (0.833 ml, 8.94 mmol) and was allowed to stir for one hour at room temperature. LC/MS showed mostly product, so the reaction mixture was concentrated. The crude residue was carried on to step 3 without purification. (M+H)+=271.2.

後処理

  1. stirringto stir for one hour at room temperature
  2. concentrationso the reaction mixture was concentrated
  3. customThe crude residue was carried on to step 3 without purification

出典と根拠

ORDレコード
ord-9393c27266bf4fdba58db712976346a9
出典データセット
uspto-grants-2015_04
特許番号
US09012443B2

反応ノート

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