Ethenamine, N,N-dimethyl-2-nitro- → 4-Ethoxycarbonyl-3-(2-nitrovinyl)indole

HRID 569043

反応式

HRID 569043 の反応式
[CH2:1]([O:3][C:4]([C:6]1[CH:14]=[CH:13][CH:12]=[C:11]2[C:7]=1[CH:8]=[CH:9][NH:10]2)=[O:5])[CH3:2].CN([CH:18]=[CH:19][N+:20]([O-:22])=[O:21])C>C(OCC(F)(F)F)(=O)C>[CH2:1]([O:3][C:4]([C:6]1[CH:14]=[CH:13][CH:12]=[C:11]2[C:7]=1[C:8]([CH:18]=[CH:19][N+:20]([O-:22])=[O:21])=[CH:9][NH:10]2)=[O:5])[CH3:2]

参加物

4

反応物 2

HCID 518458Ethenamine, N,N-dimethyl-2-nitro-HCID 605034Ethyl indole-4-carboxylate

生成物 1

HCID 540596304-Ethoxycarbonyl-3-(2-nitrovinyl)indole

試薬・触媒・溶媒 1

HCID 1362562,2,2-Trifluoroethyl Acetate溶媒

実験手順

5 g of 4-ethoxycarbonyl indole are added to a solution of 3.1 g of dimethylamino-2-nitroethylene in 20 ml of trifluoroethyl acetate refrigerated under argon. The reaction mixture is introduced into ice water after it had been standing overnight at room temperature. The aqueous phase is repeatedly extracted with ethyl acetate. The combined ethyl acetate extracts are extracted first with sodium bicarbonate solution, then a saturated sodium chloride solution, dried and evaporated. The residue is recrystallized from ethanol. Yield: 4.5 g of 4-ethoxycarbonyl-3-(2-nitrovinyl)-indole. Yellow crystals with a 197°-199° C. melting point.

後処理

  1. extractionThe aqueous phase is repeatedly extracted with ethyl acetate
  2. extractionThe combined ethyl acetate extracts are extracted first with sodium bicarbonate solution
  3. dry with materiala saturated sodium chloride solution, dried
  4. customevaporated
  5. customThe residue is recrystallized from ethanol
  6. customwith a 197°-199° C.

出典と根拠

ORDレコード
ord-6f2a0ddab3ef4b25b66fd79945d51302
出典データセット
uspto-grants-1988_03
特許番号
US04731358

関連ノート

読み込み中…