Nitric Acid → HCID 10703909、化合物

HRID 418474

反応式

HRID 418474 の反応式
[Cl:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[C:4]([CH3:11])[CH:3]=1.S(=O)(=O)(O)O.[N+:17]([O-])([OH:19])=[O:18]>>[Cl:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[C:4]([CH3:11])[C:3]=1[N+:17]([O-:19])=[O:18]

参加物

4

反応物 3

HCID 944Nitric AcidHCID 1118Sulfuric AcidHCID 3482694-Chloro-2-methylbenzoic acid

生成物 1

HCID 10703909HCID 10703909、化合物

反応条件

温度
70 °C

実験手順

A round bottom flask was charged with 4-chloro-2-methylbenzoic acid (200 mg, 0.001 mol) and sulfuric acid (1 mL, 0.02 mol). Fuming nitric acid (0.05 mL, 0.001 mol) was added at −20° C. and the reaction was stirred for 1 hour at 70° C. and poured into ice cold water, whereupon the mixture of 2- and 4-nitro compounds precipitated out. The precipitate was filtered and dissolved in ethyl acetate (30 mL) and washed with saturated aqueous sodium bicarbonate solution and brine, and dried over sodium sulfate. The solvent was reduced to ¼ volume whereby the undesired isomer precipitated out. The precipitate was filtered and the filtrate was dried to afford a 1:1 mixture of isomers as a white solid.

後処理

  1. customprecipitated out
  2. filtrationThe precipitate was filtered
  3. dissolutiondissolved in ethyl acetate (30 mL)
  4. washwashed with saturated aqueous sodium bicarbonate solution and brine
  5. dry with materialdried over sodium sulfate
  6. customprecipitated out
  7. filtrationThe precipitate was filtered
  8. customthe filtrate was dried
  9. customto afford
  10. additiona 1:1 mixture of isomers as a white solid

出典と根拠

ORDレコード
ord-e73d507498a541ee9c4d2cded8b43251
出典データセット
uspto-grants-2012_01
特許番号
US08093265B2

関連ノート

読み込み中…