Water → Methyl 3-hydroxy-5-nitrobenzoate

HRID 431384

反応式

HRID 431384 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

HCID 239344Methyl 3-hydroxy-5-nitrobenzoate

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-f874f77347bf42398aa8eee6aedda577
出典データセット
uspto-grants-2003_12
特許番号
US06656971B2

関連ノート

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