1,2-Dimethyl-3-nitrobenzene → HCID 21194232, 화합물

HRID 52161

반응식

HRID 52161 반응식
[Na].[N+:2]([C:5]1[CH:10]=[CH:9][CH:8]=[C:7]([CH3:11])[C:6]=1[CH3:12])([O-:4])=[O:3].[C:13](OCC)(=[O:19])[C:14]([O:16]CC)=[O:15].[OH-].[Na+]>O.C(O)C>[CH3:11][C:7]1[CH:8]=[CH:9][CH:10]=[C:5]([N+:2]([O-:4])=[O:3])[C:6]=1[CH2:12][C:13](=[O:19])[C:14]([OH:16])=[O:15]

참가 물질

7

반응물 4

HCID 67391,2-Dimethyl-3-nitrobenzeneHCID 7268Diethyl OxalateHCID 14798Sodium HydroxideHCID 5360545Sodium

생성물 1

HCID 21194232HCID 21194232, 화합물수율 61%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

Sodium (3.802 g, 165.38 mmol, 2.5 eq) was added portionwise into ethanol (66 mL, 1M) at 0° C. Next, 3-nitro-ortho-xylene (10.00 g, 66.15 mmol, 1 eq) and diethyl oxalate (19.33 g, 132.23 mmol, 2 eq) were added. The mixture was stirred at room temperature for 18 hours and then refluxed for 10 minutes. 1N sodium hydroxide and water were added and the reaction was stirred for one hour. The ethanol was removed under vacuum. Water was added and the aqueous solution was acidified with concentrated hydrochloric acid to ph~2. The mixture was extracted with methylene chloride. The extracts were dried (magnesium sulfate) and concentrated to give the title compound (9.0 g, 61%).

후처리

  1. temperaturerefluxed for 10 minutes
  2. stirringthe reaction was stirred for one hour
  3. customThe ethanol was removed under vacuum
  4. additionWater was added
  5. extractionThe mixture was extracted with methylene chloride
  6. dry with materialThe extracts were dried (magnesium sulfate)
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-631527924b8e4da9a6a90a47ed6c1ba9
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05616591

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