2-Nitropropane → HCID 18706556, 화합물

HRID 1422262노트

반응식

HRID 1422262 반응식
[Na].[N+](C(C)C)([O-])=[O:3].Br[CH2:9][C:10]1[CH:19]=[C:18]([Br:20])[CH:17]=[C:16]2[C:11]=1[N:12]=[C:13]([O:23][CH3:24])[C:14]([O:21][CH3:22])=[N:15]2.O>CO>[Br:20][C:18]1[CH:17]=[C:16]2[C:11]([N:12]=[C:13]([O:23][CH3:24])[C:14]([O:21][CH3:22])=[N:15]2)=[C:10]([CH:9]=[O:3])[CH:19]=1

참가 물질

6

반응물 4

HCID 3982-NitropropaneHCID 962WaterHCID 5360545SodiumHCID 23298010HCID 23298010, 화합물

생성물 1

HCID 18706556HCID 18706556, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

1.38 g (60 mmol) of sodium are dissolved in portions, at 0° C. under N2, in 200 ml of methanol. At 0° C., 5.85 ml (65 mmol) of 2-nitropropane are added dropwise. 18.1 g (50 mmol) of 5-(bromomethyl)-7-bromo-2,3-dimethoxy-quinoxaline are then added. The beige suspension is heated to reflux and stirred for 1 hour. The reaction mixture is poured onto 600 ml of water and the methanol is distilled off. The residue is extracted twice with ethyl acetate, and the organic phases are dried over sodium sulfate and filtered with suction. The filtrate is concentrated and the residue is dried under a high vacuum. 7-Bromo-5-formyl-2,3-dimethoxy-quinoxaline is obtained in the form of beige crystals having a melting point of 179-182° C.

후처리

  1. temperatureThe beige suspension is heated
  2. temperatureto reflux
  3. distillationthe methanol is distilled off
  4. extractionThe residue is extracted twice with ethyl acetate
  5. dry with materialthe organic phases are dried over sodium sulfate
  6. filtrationfiltered with suction
  7. concentrationThe filtrate is concentrated
  8. customthe residue is dried under a high vacuum

출처 및 근거

ORD 기록
ord-441da0aabcfd463781e7d010bf2ede07
출처 데이터셋
uspto-grants-2000_06
특허 번호
US06080743

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