Oxalyl chloride → 5-(4-Bromo-phenyl)-3-methyl-isoxazole-4-carbonyl chloride
反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[O:12][N:11]=[C:10]([CH3:13])[C:9]=2[C:14]([OH:16])=O)=[CH:4][CH:3]=1.C(Cl)(=O)C([Cl:20])=O>C(Cl)Cl.CN(C=O)C>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[O:12][N:11]=[C:10]([CH3:13])[C:9]=2[C:14]([Cl:20])=[O:16])=[CH:4][CH:3]=1参加物
5
実験手順
5-(4-Bromo-phenyl)-3-methyl-isoxazole-4-carboxylic acid (4.2 g, 14.89 mmol) was dissolved in CH2Cl2 (42 mL) under N2 atmosphere. Oxalyl chloride (2.6 mL, 29.78 mmol) and DMF (5 drops) were added and the reaction stirred for 2.5 hours at room temperature. Then, additional oxalyl chloride (5 mL, 57.3 mmol) was added. After 30 minutes, the reaction mixture was concentrated and placed under high vacuum. The crude material was used directly in the next step.
後処理
- waitAfter 30 minutes
- concentrationthe reaction mixture was concentrated
出典と根拠
- ORDレコード
- ord-8ee5c0a6deeb4b19ba4cfd4dfd012123
- 出典データセット
- uspto-grants-2012_07
- 特許番号
- US08217066B2
反応ノート
読み込み中…