Water → Methyl 4-hydroxy-3-iodo-5-nitrobenzoate
反応式
[OH:1][C:2]1[CH:11]=[CH:10][C:5]([C:6]([O:8][CH3:9])=[O:7])=[CH:4][C:3]=1[N+:12]([O-:14])=[O:13].[I:15]Cl.O>C(O)(=O)C>[OH:1][C:2]1[C:3]([N+:12]([O-:14])=[O:13])=[CH:4][C:5]([C:6]([O:8][CH3:9])=[O:7])=[CH:10][C:11]=1[I:15]参加物
5
反応条件
- 温度
- 100 °C
実験手順
To a solution of methyl 4-hydroxy-3-nitrobenzoate (2.0 g) in acetic acid (15 mL) was added iodine monochloride (1.65 mg) in acetic acid, and the mixture was stirred at 100° C. for 1.5 h. After cooling to room temperature, the mixture was poured into water (200 mL), and stirred for 30 min. The mixture was filtered and washed with water and hexanes. The yellow powder was collected by filtration and dried in vacuum oven overnight to give 2.99 g of the title compound: 1H NMR (300 MHz, CDCl3) δ 11.68, 8.81, 8.72, 3.96.
後処理
- temperatureAfter cooling to room temperature
- stirringstirred for 30 min
- filtrationThe mixture was filtered
- washwashed with water and hexanes
- filtrationThe yellow powder was collected by filtration
- customdried in vacuum oven overnight
出典と根拠
- ORDレコード
- ord-c1dd2980181a479f9a861aa29f4deeb3
- 出典データセット
- uspto-grants-2010_06
- 特許番号
- US07727997B2
反応ノート
読み込み中…