Water → Methyl 4-hydroxy-3-iodo-5-nitrobenzoate

HRID 14183

反応式

HRID 14183 の反応式
[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

反応物 3

HCID 962WaterHCID 24640Iodine chlorideHCID 66835Benzoic acid, 4-hydroxy-3-nitro-, methyl ester

生成物 1

HCID 21086206Methyl 4-hydroxy-3-iodo-5-nitrobenzoate収率 91,075.398%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒2 回

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

  1. temperatureAfter cooling to room temperature
  2. stirringstirred for 30 min
  3. filtrationThe mixture was filtered
  4. washwashed with water and hexanes
  5. filtrationThe yellow powder was collected by filtration
  6. 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

関連ノート

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