Water → Methyl 3-hydroxy-5-nitrobenzoate

HRID 431384노트

반응식

HRID 431384 반응식
[OH:1][C:2]1[CH:3]=[C:4]([CH:8]=[C:9]([N+:11]([O-:13])=[O:12])[CH:10]=1)[C:5]([OH:7])=[O:6].S(=O)(=O)(O)O.[C:19]([O-])([O-])=O.[Na+].[Na+].O>CO>[OH:1][C:2]1[CH:3]=[C:4]([CH:8]=[C:9]([N+:11]([O-:13])=[O:12])[CH:10]=1)[C:5]([O:7][CH3:19])=[O:6]

참가 물질

6

반응물 4

HCID 962WaterHCID 1118Sulfuric AcidHCID 10340Sodium CarbonateHCID 8203933-Hydroxy-5-nitrobenzoic acid

생성물 1

HCID 239344Methyl 3-hydroxy-5-nitrobenzoate

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A solution of 3-hydroxy-5-nitrobenzoic acid (2.00 g, 11 mmol) and concentrated sulfuric acid (0.5 mL) in MeOH (15 mL) was refluxed overnight, cooled to room temperature, and poured into mixture of Na2CO3 (saturated solution, 25 mL), water (150 mL), and ice (50 g). Resulting precipitate was filtered, washed with water (3×30 mL), and air-dried. Yellow microcrystals, yield 1.37 g (63%). 1H NMR (DMSO-d6, 400 MHz), δ: 10.94 (s, 1H); 8.09 (s, 1H); 7.78 (s, 1H); 7.71 (s, 1H); 3.90 (s, 3H).

후처리

  1. customResulting precipitate
  2. filtrationwas filtered
  3. washwashed with water (3×30 mL)
  4. customair-dried

출처 및 근거

ORD 기록
ord-f874f77347bf42398aa8eee6aedda577
출처 데이터셋
uspto-grants-2003_12
특허 번호
US06656971B2

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