Hydrochloric Acid → Ethyl α-(hydroxyimino)-2-nitrobenzeneacetate

HRID 1721812노트

반응식

HRID 1721812 반응식
[N+:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[CH2:10][C:11]([O:13][CH2:14][CH3:15])=[O:12])([O-:3])=[O:2].[N:16](OCCC(C)C)=[O:17].[O-]CC.[Na+].[Na].Cl>C(O)C.O>[N+:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[C:10](=[N:16][OH:17])[C:11]([O:13][CH2:14][CH3:15])=[O:12])([O-:3])=[O:2]

참가 물질

8

반응물 5

HCID 313Hydrochloric AcidHCID 8053Isoamyl NitriteHCID 595882Ethyl 2-nitrophenylacetateHCID 2723922Sodium ethoxideHCID 5360545Sodium

생성물 1

HCID 53403224Ethyl α-(hydroxyimino)-2-nitrobenzeneacetate

시약·촉매·용매 2

HCID 702Ethanol용매3회HCID 962Water용매

실험 절차

A mixture of 50 g of ethyl (2-nitrophenyl)acetate, 30 g of isoamyl nitrite and 400 ml of ethanol was added to sodium ethoxide prepared by treating 5.1 g of sodium with 100 ml of ethanol and diluting with ethanol to 100 ml. The mixture was heated at 50°-60° C. for 4 hours, cooled, 400 ml of water was added, the mixture was acidified with 6N hydrochloric acid and extracted with ether. The extract was stripped of solvent, and the residue was recrystallized from benzene to give ethyl (2-nitrophenyl)glyoxylate oxime (3A), as a white solid, m.p.: 167°-168° C.

후처리

  1. customprepared
  2. temperatureThe mixture was heated at 50°-60° C. for 4 hours
  3. temperaturecooled
  4. extractionextracted with ether
  5. customthe residue was recrystallized from benzene

출처 및 근거

ORD 기록
ord-ee7926cc2ef44d1288995b7421883d16
출처 데이터셋
uspto-grants-1989_08
특허 번호
US04853027

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