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2-Butanamine, 2-methyl- → 6,7-dichloro-2,3-dimethoxy-5-{[2-(N-(1,1-dimethylpropyl)amino)ethyl]pyrazol-1-ylmethyl}quinoxaline

HRID 1957114
ノート
印刷プレビュー

反応式

HRID 1957114 の反応式
Cl[CH2:2][CH2:3][CH:4]([N:21]1[CH:25]=[CH:24][CH:23]=[N:22]1)[C:5]1[C:14]([Cl:15])=[C:13]([Cl:16])[CH:12]=[C:11]2[C:6]=1[N:7]=[C:8]([O:19][CH3:20])[C:9]([O:17][CH3:18])=[N:10]2.[CH3:26][C:27]([NH2:31])([CH3:30])[CH2:28][CH3:29]>C(O)C>[Cl:15][C:14]1[C:5]([CH:4]([CH2:3][CH2:2][NH:31][C:27]([CH3:30])([CH3:26])[CH2:28][CH3:29])[N:21]2[CH:25]=[CH:24][CH:23]=[N:22]2)=[C:6]2[C:11](=[CH:12][C:13]=1[Cl:16])[N:10]=[C:9]([O:17][CH3:18])[C:8]([O:19][CH3:20])=[N:7]2
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 689862-Butanamine, 2-methyl-HCID 543391965-[(2-Chloroethyl)pyrazol-1-ylmethyl]-6,7-dichloro-2,3-dimethoxyquinoxaline

生成物 1

HCID 232249886,7-dichloro-2,3-dimethoxy-5-{[2-(N-(1,1-dimethylpropyl)amino)ethyl]pyrazol-1-ylmethyl}quinoxaline収率 38%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
105 °C

実験手順

A mixture of 5-[(2-chloroethyl)pyrazol-1-ylmethyl]-6,7-dichloro-2,3-dimethoxyquinoxaline (150 mg, 0.37 mmol), 1,1-dimethyl-1-propylamine (3 mL) and ethanol (5 mL) were heated in a closed vessel at 105° C. for 7 hours. The mixture was cooled, the solvent was removed under reduced pressure, and the residue was dissolved in ethyl acetate (75 mL). The solution was washed with saturated aqueous sodium bicarbonate, dried (MgSO4) and concentrated under reduced pressure. Purification by flash chromatography (elution with dichloromethane, then an ethyl acetate/methanol/triethylamine gradient) gave 6,7-dichloro-2,3-dimethoxy-5-{[2-(N-(1,1-dimethylpropyl)amino)ethyl]pyrazol-1-ylmethyl}quinoxaline (65 mg, 38%), as a pale yellow solid.

後処理

  1. temperatureThe mixture was cooled
  2. customthe solvent was removed under reduced pressure
  3. dissolutionthe residue was dissolved in ethyl acetate (75 mL)
  4. washThe solution was washed with saturated aqueous sodium bicarbonate
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated under reduced pressure
  7. customPurification by flash chromatography (
  8. washelution with dichloromethane

出典と根拠

ORDレコード
ord-7e8695b6787e4c51a6b28f32700ac456
出典データセット
uspto-grants-1998_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05783572

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート