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

HRID 1899916

反応式

HRID 1899916 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-a076b1984e00425fb2c2e48d60d26175
出典データセット
uspto-grants-1996_11
特許番号
US05574038

関連ノート

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