Propionic anhydride → 6-chloro-2-ethyl-1H-imidazo[4,5-b]quinoxaline

HRID 1581127노트

반응식

HRID 1581127 반응식
[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.[C:14](OC(=O)CC)(=O)[CH2:15][CH3:16]>C(O)(=O)CC>[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[N:8]=[C:7]1[NH:12][C:14]([CH2:15][CH3:16])=[N:13][C:6]1=[N:5]2

참가 물질

4

반응물 2

HCID 31263Propionic anhydrideHCID 125173906-Chloroquinoxaline-2,3-diamine

생성물 1

HCID 1784375416-chloro-2-ethyl-1H-imidazo[4,5-b]quinoxaline수율 88.1%

시약·촉매·용매 1

HCID 1032Propionic Acid용매

실험 절차

78 G (0.4 mole) of 6-chloro-2,3-diamino-quinoxaline were dissolved in 500 ml of anhydrous propionic acid and 105 g (0.8 mole) of propionic anhydride were added thereto. The reaction mixture was heated to the boil under reflux for 5 hours. After cooling, the solvent was distilled off in vacuo, the residue was taken up in dilute sodium hydroxide solution, the mixture was filtered, the filtrate was acidified with dilute hydrochloric acid and the resulting precipitate was filtered off. It was well washed with water and dried in vacuo at 110°C. 82 g (representing 88% of theory) of 6-chloro-2-ethyl-1H-imidazo[4,5-b]quinoxaline of melting point 190°C (decomposition) were obtained.

후처리

  1. temperatureThe reaction mixture was heated to the boil
  2. temperatureunder reflux for 5 hours
  3. temperatureAfter cooling
  4. distillationthe solvent was distilled off in vacuo
  5. filtrationthe mixture was filtered
  6. filtrationthe resulting precipitate was filtered off
  7. washIt was well washed with water
  8. customdried in vacuo at 110°C

출처 및 근거

ORD 기록
ord-4bd62135f66047e2a7e1e1aa37a7afa4
출처 데이터셋
uspto-grants-1976_01
특허 번호
US03935312

반응 노트

불러오는 중…