Oxalic Acid → 6-Bromo-8-methyl-1,4,7,8,9,10-hexahydro-pyrido[4,3-f]quinoxaline-2,3-dione

HRID 48207ノート

反応式

HRID 48207 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([NH2:14])[C:5]([NH2:13])=[C:6]2[C:11]=1[CH2:10][N:9]([CH3:12])[CH2:8][CH2:7]2.[C:15](O)(=[O:19])[C:16](O)=[O:17]>Cl>[Br:1][C:2]1[C:11]2[CH2:10][N:9]([CH3:12])[CH2:8][CH2:7][C:6]=2[C:5]2[NH:13][C:15](=[O:19])[C:16](=[O:17])[NH:14][C:4]=2[CH:3]=1

参加物

4

反応物 2

HCID 971Oxalic AcidHCID 103550328-Bromo-1,2,3,4-tetrahydro-2-methyl-5,6-isoquinolinediamine

生成物 1

HCID 98181346-Bromo-8-methyl-1,4,7,8,9,10-hexahydro-pyrido[4,3-f]quinoxaline-2,3-dione収率 24.1%

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

A solution of the product from Example 13 (0.62 g, 2.56 mmol) and oxalic acid (0.23 g, 2.56 mmol) in 25 mL of 3N aqueous HCl solution were heated at reflux for 18 hours. The reaction mixture was cooled to room temperature and the solid which formed was collected by filtration and washed with cold water. The solid was recrystallized from hot water and dried under vacuum (100° C., P2O5) to give the title compound as a tan solid (0.191 g, 20%), mp=315-320° C. (dec.).

後処理

  1. temperatureat reflux for 18 hours
  2. customthe solid which formed
  3. filtrationwas collected by filtration
  4. washwashed with cold water
  5. customThe solid was recrystallized from hot water
  6. dry with materialdried under vacuum (100° C., P2O5)

出典と根拠

ORDレコード
ord-28485785eeb5490989bcf2076b9474c3
出典データセット
uspto-grants-2004_03
特許番号
US06703391B2

反応ノート

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