N-(2-acetyl-4-bromophenyl)acetamide → 6-Bromo-2,4-dimethylquinazoline

HRID 1496855

반응식

HRID 1496855 반응식
[C:1]([C:4]1[CH:9]=[C:8]([Br:10])[CH:7]=[CH:6][C:5]=1[NH:11][C:12](=O)[CH3:13])(=O)[CH3:2].C([O-])(=O)C.[NH4+:19]>C(O)(=O)C>[Br:10][C:8]1[CH:9]=[C:4]2[C:5](=[CH:6][CH:7]=1)[N:11]=[C:12]([CH3:13])[N:19]=[C:1]2[CH3:2]

참가 물질

4

반응물 2

HCID 459291N-(2-acetyl-4-bromophenyl)acetamideHCID 517165Ammonium Acetate

생성물 1

HCID 583293276-Bromo-2,4-dimethylquinazoline수율 23.4%

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
100 °C

실험 절차

415 mg N-(2-acetyl-4-bromophenyl)acetamide and 0.624 g of ammonium acetate was dissolved in 5 mL of glacial acetic acid and heated for 2 days at 100° C. The solvent was removed and the residue suspended in water and extracted with DCM. The organic phase was concentrated and purified via FCC (25 g SiO2, DCM:MeOH 100:0→70:30) to yield 90 mg of 6-bromo-2,4-dimethylquinazoline as oil. Analysis: HPLC-MS: Rt=1.26 min (method V003—003), M+H=237/239.

후처리

  1. customThe solvent was removed
  2. extractionextracted with DCM
  3. concentrationThe organic phase was concentrated
  4. custompurified via FCC (25 g SiO2, DCM:MeOH 100:0→70:30)

출처 및 근거

ORD 기록
ord-be0150cd47cd4957a9fe924c07924e25
출처 데이터셋
uspto-grants-2015_12
특허 번호
US09199937B2

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