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

HRID 1473664노트

반응식

HRID 1473664 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-9393c27266bf4fdba58db712976346a9
출처 데이터셋
uspto-grants-2015_04
특허 번호
US09012443B2

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