Ethyl iodoacetate → HCID 19958587、化合物

HRID 373768ノート

反応式

HRID 373768 の反応式
[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

参加物

4

反応物 2

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

生成物 1

HCID 19958587HCID 19958587、化合物収率 85%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-f8d086ae913e4bd7b81399eccba134ce
出典データセット
uspto-grants-1992_11
特許番号
US05166155

反応ノート

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