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

HRID 1736670

반응식

HRID 1736670 반응식
[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

참가 물질

4

반응물 2

HCID 755072-Hydroxy-6-chloroquinoxalineHCID 4311764Sodium borohydride

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-334564f7229047d3a4d3cb41d1f0a55e
출처 데이터셋
uspto-grants-1996_07
특허 번호
US05541324

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