Oxalic Acid → HCID 15524196、化合物

HRID 1106432ノート

反応式

HRID 1106432 の反応式
[Br:1][C:2]1[CH:11]=[C:10]([N+:12]([O-])=O)[C:9]([NH2:15])=[C:8]2[C:3]=1[CH2:4][CH2:5][N:6]([CH2:16][CH2:17][CH2:18][C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)[CH2:7]2.[C:25](O)(=[O:29])[C:26](O)=[O:27]>Cl>[Br:1][C:2]1[C:3]2[CH2:4][CH2:5][N:6]([CH2:16][CH2:17][CH2:18][C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)[CH2:7][C:8]=2[C:9]2[NH:15][C:25](=[O:29])[C:26](=[O:27])[NH:12][C:10]=2[CH:11]=1

参加物

4

反応物 2

HCID 971Oxalic AcidHCID 155241945-Bromo-1,2,3,4-tetrahydro-7-nitro-2-(3-phenylpropyl)-8-isoquinolinamine

生成物 1

HCID 15524196HCID 15524196、化合物収率 60.3%

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

A solution of the product from Example 12 (0.98 g, 2.72 mmol) in 3N HCl (35 mL) was treated with oxalic acid (0.36 g, 2.86 mmol) and refluxed for five hours. When cool to room temperatures the precipitate was filtered, suspended in water (70 mL) and basifyed to pH 8. The solids were filtered, and dried to give the title compound (0.68 g, 60%) as a brown solid, mp=288-293° C.

後処理

  1. temperaturerefluxed for five hours
  2. temperatureWhen cool to room temperatures the precipitate
  3. filtrationwas filtered
  4. filtrationThe solids were filtered
  5. customdried

出典と根拠

ORDレコード
ord-ebeecbeca3644c59b97b3ab96acdbe55
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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