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

HRID 348974

반응식

HRID 348974 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

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 176Acetic Acid용매2회

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

  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

출처 및 근거

ORD 기록
ord-ce3a917d547b4565ad207f5df577f15f
출처 데이터셋
uspto-grants-2007_02
특허 번호
US07176242B2

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