Nitric Acid → HCID 10703909, 화합물

HRID 418474

반응식

HRID 418474 반응식
[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]

참가 물질

4

반응물 3

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

생성물 1

HCID 10703909HCID 10703909, 화합물

반응 조건

온도
70 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-e73d507498a541ee9c4d2cded8b43251
출처 데이터셋
uspto-grants-2012_01
특허 번호
US08093265B2

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