Pyridine → 6-Chloro-2,3-bis-(valeramido)quinoxaline

HRID 1288223ノート

反応式

HRID 1288223 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[N:8]=[C:7]([NH2:12])[C:6]([NH2:13])=[N:5]2.N1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1.[C:20](Cl)(=[O:25])[CH2:21][CH2:22][CH2:23][CH3:24].[O:27]1CCCC1>O>[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[N:8]=[C:7]([NH:12][C:15](=[O:27])[CH2:16][CH2:17][CH2:18][CH3:19])[C:6]([NH:13][C:20](=[O:25])[CH2:21][CH2:22][CH2:23][CH3:24])=[N:5]2

参加物

6

反応物 4

HCID 1049PyridineHCID 8028TetrahydrofuranHCID 61186Valeryl chlorideHCID 125173906-Chloroquinoxaline-2,3-diamine

生成物 1

HCID 215045946-Chloro-2,3-bis-(valeramido)quinoxaline

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A suspension of 100 parts of 6-chloro-2,3-diaminoquinoxaline in 1000 parts of pyridine was cooled to 5° in an ice bath. A solution of 152 parts of valeryl chloride in 130 parts of tetrahydrofuran was added quickly with good cooling to prevent the temperature from rising above 20°. The reaction mixture was stirred at ambient temperature for 1 hour and then poured into 2500 parts of water. The solid which separated was removed by filtration and washed with water, methanol, and then ether. The crude product was recrystallized from methanol to yield 55 parts of 6-chloro-2,3-bis-(valeramido)quinoxaline, m.p. 171°-173°, as a colorless solid.

後処理

  1. temperaturewas cooled to 5° in an ice bath
  2. temperaturewith good cooling
  3. customfrom rising above 20°
  4. customThe solid which separated
  5. customwas removed by filtration
  6. washwashed with water, methanol
  7. customThe crude product was recrystallized from methanol

出典と根拠

ORDレコード
ord-1c884f5958454788aaa90f22eeeb7d52
出典データセット
uspto-grants-1976_10
特許番号
US03987171

反応ノート

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