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

HRID 569043

반응식

HRID 569043 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 1362562,2,2-Trifluoroethyl Acetate용매

실험 절차

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.

후처리

  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.

출처 및 근거

ORD 기록
ord-6f2a0ddab3ef4b25b66fd79945d51302
출처 데이터셋
uspto-grants-1988_03
특허 번호
US04731358

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