Dimethylformamide → 2,5-Dichloro-3-nitrobenzoic acid

HRID 1759263

반응식

HRID 1759263 반응식
[Cl:1][C:2]1[C:10]([N+:11]([O-:13])=[O:12])=[C:9](C(O)=O)[C:8]([Cl:17])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].CN(C)C=O>>[Cl:1][C:2]1[C:10]([N+:11]([O-:13])=[O:12])=[CH:9][C:8]([Cl:17])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5]

참가 물질

3

반응물 2

HCID 6228DimethylformamideHCID 2809622,5-Dichloro-3-nitrobenzene-1,4-dicarboxylic acid

생성물 1

HCID 69512,5-Dichloro-3-nitrobenzoic acid

실험 절차

0.0008 moles of 2,5-dichloro-3-nitro-terephthalic acid were refluxed for 1 hour in 0.334 moles of dimethyl formamide (DMF), after which time the reaction mixture was flash evaporated to remove most of the DMF. To the residue was added 60 ml of water with agitation, and an orange precipitate formed which was filtered off and washed. The precipitate was dissolved in approximately 50 ml of saturated sodium bicarbonate solution, refiltered and then extracted with chloroform. The aqueous phase was acidified with 10% hydrochloric acid to complete precipitation, and the resulting precipitate was filtered, washed and dried to give an 85% crude yield of 2,5-dichloro-3-nitro-benzoic acid. Subsequent GLC analysis showed it to be 95.8% pure; thus, the yield of the process was 79.5% of theoretical.

후처리

  1. customevaporated
  2. customto remove most of the DMF
  3. additionTo the residue was added 60 ml of water with agitation
  4. customan orange precipitate formed which
  5. filtrationwas filtered off
  6. washwashed
  7. dissolutionThe precipitate was dissolved in approximately 50 ml of saturated sodium bicarbonate solution
  8. extractionextracted with chloroform
  9. customprecipitation
  10. filtrationthe resulting precipitate was filtered
  11. washwashed
  12. customdried

출처 및 근거

ORD 기록
ord-2880f4b0e0064a68bf6a559fd7ca5a71
출처 데이터셋
uspto-grants-1982_07
특허 번호
US04339601

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