2-Hydroxy-6-chloroquinoxaline → 6-chloro-3,4-dihydroquinoxalin-2(1h)-one

HRID 1736670

反応式

HRID 1736670 の反応式
[BH4-].[Na+].[Cl:3][C:4]1[CH:5]=[C:6]2[C:11](=[CH:12][CH:13]=1)[NH:10][C:9](=[O:14])[CH:8]=[N:7]2>C(O)C>[Cl:3][C:4]1[CH:5]=[C:6]2[C:11](=[CH:12][CH:13]=1)[NH:10][C:9](=[O:14])[CH2:8][NH:7]2

参加物

4

反応物 2

HCID 755072-Hydroxy-6-chloroquinoxalineHCID 4311764Sodium borohydride

生成物 1

HCID 2835276-chloro-3,4-dihydroquinoxalin-2(1h)-one

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Sodium borohydride (5.10 g) is added to a mixture of 6-chloro-1,2-dihydroquinoxalin-2-one (5.60 g), and ethanol (200 ml). The resultant solution is stirred for 2.5 hr at 20°-25°. The material is partitioned between water and ethyl acetate, the phases are separated, the organic phase is dried over magnesium sulfate and concentrated under reduced pressure to give a solid which is recrystallized from ethyl acetate/hexane to give the title compound, mp 171-174° ; IR (mineral oil) 2953, 2925, 1687, 1517, 1408, 1307 and 1299 cm-1 ; NMR (CDCl3 -MeOD) 6.6-6.8 and 3.95 δ; MS (m/z) 182, 153.

後処理

  1. customThe material is partitioned between water and ethyl acetate
  2. customthe phases are separated
  3. dry with materialthe organic phase is dried over magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customto give a solid which
  6. customis recrystallized from ethyl acetate/hexane

出典と根拠

ORDレコード
ord-334564f7229047d3a4d3cb41d1f0a55e
出典データセット
uspto-grants-1996_07
特許番号
US05541324

関連ノート

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