Ethyl iodoacetate → HCID 19958587, 화합물

HRID 373768노트

반응식

HRID 373768 반응식
[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][C:11]=1[Cl:12])[NH:8][C:7](=[O:13])[CH:6]=[N:5]2.I[CH2:15][C:16]([O:18][CH2:19][CH3:20])=[O:17]>C(O)C>[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][C:11]=1[Cl:12])[N:8]([CH2:15][C:16]([O:18][CH2:19][CH3:20])=[O:17])[C:7](=[O:13])[CH:6]=[N:5]2

참가 물질

4

반응물 2

HCID 12183Ethyl iodoacetateHCID 144236366,7-Dichloroquinoxalin-2(1H)-one

생성물 1

HCID 19958587HCID 19958587, 화합물수율 85%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Under a nitrogen atmosphere Na (0.25 g, 11 mmol) was dissolved in 100 ml of abs. ethanol and 6,7-dichloroquinoxalin-2(1H)-one (2.15 g, 10 mmol) (Liebigs Ann. Chem., (1982), 754) was added. The mixture was refluxed for 30 min., cooled to room temperature, and ethyl iodoacetate (1.43 ml, 12 mmol) was added. The clear reaction mixture was refluxed for 2 h during which time a precipitate was formed. This was filtered off, washed with abs. ethanol and dried to afford 2.56 g (85%) of 6,7-dichloro-1-ethoxycarbonylmethylquinoxalin-2(1H)-one. 1H-NMR (DMSO-d6):δ1.23 (t, 3H), 4.20 (q, 2H), 5.08 (s, 2H), 8.05 (s, 1H), 8.17 (s, 1H), 8.38 (s, 1H).

후처리

  1. temperatureThe mixture was refluxed for 30 min.
  2. temperatureThe clear reaction mixture was refluxed for 2 h during which time a precipitate
  3. customwas formed
  4. filtrationThis was filtered off
  5. washwashed with abs
  6. dry with materialethanol and dried

출처 및 근거

ORD 기록
ord-f8d086ae913e4bd7b81399eccba134ce
출처 데이터셋
uspto-grants-1992_11
특허 번호
US05166155

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