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

HRID 1721812ノート

反応式

HRID 1721812 の反応式
[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]

参加物

8

反応物 5

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒3 回HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-ee7926cc2ef44d1288995b7421883d16
出典データセット
uspto-grants-1989_08
特許番号
US04853027

反応ノート

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