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

HRID 1402702

反応式

HRID 1402702 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

HCID 583293276-Bromo-2,4-dimethylquinazoline収率 23.4%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
100 °C

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-8a7033eb63044ca2be9855fcfbe6a4ac
出典データセット
uspto-grants-2014_12
特許番号
US08912173B2

関連ノート

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