Phosphorus oxychloride → 2-Chloro-5,6,7,8-tetrahydroquinoxaline

HRID 1789996노트

반응식

HRID 1789996 반응식
[NH:1]1[C:10]2[CH2:9][CH2:8][CH2:7][CH2:6][C:5]=2[N:4]=[CH:3][C:2]1=O.P(Cl)(Cl)([Cl:14])=O>>[Cl:14][C:2]1[CH:3]=[N:4][C:5]2[CH2:6][CH2:7][CH2:8][CH2:9][C:10]=2[N:1]=1

참가 물질

3

반응물 2

HCID 24813Phosphorus oxychlorideHCID 8202241,2,5,6,7,8-Hexahydroquinoxalin-2-one

생성물 1

HCID 220369342-Chloro-5,6,7,8-tetrahydroquinoxaline수율 86%

실험 절차

A mixture of 5,6,7,8-tetrahydro-2(1H)-quinoxalinone in phosphoryl chloride (200 ml) was stirred and refluxed for 3 hours. The solvent was evaporated. The residue was taken up in ice and CH2Cl2. The mixture was basified with NH4OH. The organic layer was separated, dried (MgSO4), filtered and the solvent was evaporated, yielding 34 g (86%) of 2-chloro-5,6,7,8-tetrahydroquinoxaline (interm. 3).

후처리

  1. temperaturerefluxed for 3 hours
  2. customThe solvent was evaporated
  3. customThe organic layer was separated
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. customthe solvent was evaporated

출처 및 근거

ORD 기록
ord-fbaa14d6e4c243d89586713fa1c24c59
출처 데이터셋
uspto-grants-2006_07
특허 번호
US07071192B1

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