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

HRID 1106426ノート

反応式

HRID 1106426 の反応式
[Br:1][C:2]1[CH:11]=[C:10]([NH2:12])[C:9]([NH2:13])=[C:8]2[C:3]=1[CH2:4][CH2:5][N:6]([CH2:14][C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)[CH2:7]2.[C:21](O)(=[O:25])[C:22](O)=[O:23]>Cl>[Br:1][C:2]1[C:3]2[CH2:4][CH2:5][N:6]([CH2:14][C:15]3[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=3)[CH2:7][C:8]=2[C:9]2[NH:13][C:21](=[O:25])[C:22](=[O:23])[NH:12][C:10]=2[CH:11]=1

参加物

4

反応物 2

HCID 971Oxalic AcidHCID 155241895-Bromo-1,2,3,4-tetrahydro-2-(phenylmethyl)-7,8-isoquinolinediamine

生成物 1

HCID 155241906-Bromo-1,4,7,8,9,10-hexahydro-9-(phenylmethyl)pyrido[3,4-f]quinoxaline-2,3-dione収率 89%

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

A solution of the product from Example 7 (0.64 g, 1.93 mmol) in 3N HCl (25 mL) was treated with oxalic acid (0.37 g, 2.9 mmol) and refluxed for four hours. When cool to room temperature the precipitate was filtered, suspended in water (70 mL) and basifyed to pH 10. The solids were filtered, and dried to give the title compound (0.57 g, 89%) as a light brown solid, mp=297-302° C.

後処理

  1. temperaturerefluxed for four hours
  2. filtrationwas filtered
  3. filtrationThe solids were filtered
  4. customdried

出典と根拠

ORDレコード
ord-6b87b5aeaa6a49b2a322324572935068
出典データセット
uspto-grants-2000_05
特許番号
US06057313

反応ノート

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