2-羟基-6-氯喹喔啉 → 6-氯-3,4-二氢喹喔啉-2(1H)-酮

HRID 1378728

反应方程式

HRID 1378728 反应方程式
[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

参与物

4

反应物 2

HCID 755072-羟基-6-氯喹喔啉HCID 4311764硼氢化钠

产物 1

HCID 2835276-氯-3,4-二氢喹喔啉-2(1H)-酮

试剂、催化剂与溶剂 1

HCID 702乙醇溶剂

实验过程

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.

后处理

  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

来源与证据

ORD记录
ord-f7e7c2d8e1cb4d019ba2b747b8d2818e
来源数据集
uspto-grants-1997_09
专利号
US05668282

关联笔记

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