N-Benzylacetamide → 3-benzyl-7-chloro-2-methylquinazolin-4(3H)-one

HRID 547452

反応式

HRID 547452 の反応式
[NH2:1][C:2]1[CH:10]=[C:9]([Cl:11])[CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=O.[CH2:12]([NH:19][C:20](=O)[CH3:21])[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1>P(Cl)(Cl)(Cl)=O>[CH2:12]([N:19]1[C:4](=[O:6])[C:3]2[C:2](=[CH:10][C:9]([Cl:11])=[CH:8][CH:7]=2)[N:1]=[C:20]1[CH3:21])[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1

参加物

4

反応物 2

HCID 11500N-BenzylacetamideHCID 666462-Amino-4-chlorobenzoic acid

生成物 1

HCID 583781963-benzyl-7-chloro-2-methylquinazolin-4(3H)-one

試薬・触媒・溶媒 1

HCID 24813Phosphorus oxychloride溶媒

実験手順

2-Amino-4-chlorobenzoic acid (250 mg, 1 eq.) and N-benzylacetamide (261 mg, 1.2 eq.) were dissolved in phosphorus oxychloride (2 ml). The reaction was placed in the microwave for 10 minutes at 150° C. The reaction was quenched by pouring the mixture into ice. The crude product was extracted into ethyl acetate. The ethyl acetate layer was washed with water, 10% aqueous sodium hydroxide, dried with magnesium sulfate, filtered, and concentrated to yield 3-benzyl-7-chloro-2-methylquinazolin-4 (3H)-one as an orange solid.

後処理

  1. customThe reaction was quenched
  2. additionby pouring the mixture into ice
  3. extractionThe crude product was extracted into ethyl acetate
  4. washThe ethyl acetate layer was washed with water, 10% aqueous sodium hydroxide
  5. dry with materialdried with magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-6d9d58d3257b4282bb0988a4d0392c84
出典データセット
uspto-grants-2011_05
特許番号
US07939539B2

関連ノート

読み込み中…