Water → Methyl 4-hydroxy-3-iodo-5-nitrobenzoate
반응식
[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]참가 물질
5
반응 조건
- 온도
- 100 °C
실험 절차
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.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-c1dd2980181a479f9a861aa29f4deeb3
- 출처 데이터셋
- uspto-grants-2010_06
- 특허 번호
- US07727997B2
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