3,4-Dimethylbenzoic acid → 3,4-Dimethyl-5-nitrobenzoic acid

HRID 536430

반응식

HRID 536430 반응식
[CH3:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[CH3:11])[C:5]([OH:7])=[O:6].[N:12]([O-:14])=[O:13].[K+]>S(=O)(=O)(O)O>[CH3:1][C:2]1[CH:3]=[C:4]([CH:8]=[C:9]([N+:12]([O-:14])=[O:13])[C:10]=1[CH3:11])[C:5]([OH:7])=[O:6]

참가 물질

4

반응물 2

HCID 120733,4-Dimethylbenzoic acidHCID 516910Potassium nitrite

생성물 1

HCID 113675723,4-Dimethyl-5-nitrobenzoic acid수율 48.1%

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매2회

실험 절차

A solution of 3,4-dimethylbenzoic acid (40 g) in concentrated sulphuric acid (250 ml) was cooled to 0° C., treated with a solution of potassium nitrite (27 g) in sulphuric acid (100 ml) dropwise over a period of 1 h, and stirred for 2 h. The reaction mixture was quenched with ice cooled water (100 ml). The solid precipitated was filtered, dissolved in water (2 l), basified with 2N aqueous sodium hydroxide. The solution was acidified to pH 4 with 2N aqueous hydrochloric acid and filtered to get 3,4-dimethyl-5-nitrobenzoic acid (II) (25 g) as colorless solid. The filtrate was further acidified to pH 3 and filtered get 3,4-dimethyl-2-nitrobenzoic acid (I) (13 g) as colorless solid.

후처리

  1. customThe reaction mixture was quenched with ice
  2. temperaturecooled water (100 ml)
  3. customThe solid precipitated
  4. filtrationwas filtered
  5. dissolutiondissolved in water (2 l)
  6. filtrationfiltered

출처 및 근거

ORD 기록
ord-c0cac1017daf4671a2aa47d3bf6ad083
출처 데이터셋
uspto-grants-2014_10
특허 번호
US08859592B2

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