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

HRID 2217296ノート

反応式

HRID 2217296 の反応式
[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

参加物

3

反応物 2

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

生成物 1

HCID 220369342-Chloro-5,6,7,8-tetrahydroquinoxaline収率 86%

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-397cd1b96a6b4be38fc7ecd96ca7ec07
出典データセット
uspto-grants-2008_08
特許番号
US07407969B2

反応ノート

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