Hydrochloric Acid → 3-Hydroxy-2-nitrobenzoic acid

HRID 415161

反応式

HRID 415161 の反応式
Cl[C:2]1[C:3]([N+:11]([O-:13])=[O:12])=[C:4]([CH:8]=[CH:9][CH:10]=1)[C:5]([OH:7])=[O:6].[OH-:14].[K+].Cl>O>[OH:14][C:2]1[C:3]([N+:11]([O-:13])=[O:12])=[C:4]([CH:8]=[CH:9][CH:10]=1)[C:5]([OH:7])=[O:6]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14797Potassium HydroxideHCID 209023-Chloro-2-nitrobenzoic acid

生成物 1

HCID 2932913-Hydroxy-2-nitrobenzoic acid収率 150.2%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 3-chloro-2-nitrobenzoic acid (40 g, 0.20 mol) and KOH (160 g, 2.86 mol) in water (200 mL) was heated to reflux for 16 hr. 6N aqueous hydrochloric acid was added to the mixture to pH=3, then extracted with ethyl acetate (500 mL×4). The combined organic layers were washed with brine, dried over anhydrous sodium sulfate, and concentrated to give 3-hydroxy-2-nitrobenzoic acid (55 g), LC-MS (ESI) m/z 184 [M+1]−.

後処理

  1. temperaturewas heated
  2. temperatureto reflux for 16 hr
  3. extractionextracted with ethyl acetate (500 mL×4)
  4. washThe combined organic layers were washed with brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-f5de328daff54048ac75d1f6e3803ac8
出典データセット
uspto-grants-2012_01
特許番号
US08088760B2

関連ノート

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