Hydrochloric Acid → Methyl (2S)-4-((3-chloro-7-methoxyquinoxalin-2-yl)oxy)pyrrolidine-2-carboxylate hydrochloride

HRID 659827ノート

反応式

HRID 659827 の反応式
[Cl:1][C:2]1[C:3]([O:14][C@H:15]2[CH2:19][N:18](C(OC(C)(C)C)=O)[C@H:17]([C:27]([O:29][CH3:30])=[O:28])[CH2:16]2)=[N:4][C:5]2[C:10]([N:11]=1)=[CH:9][CH:8]=[C:7]([O:12][CH3:13])[CH:6]=2.Cl.O1CCOCC1>C(Cl)Cl>[ClH:1].[Cl:1][C:2]1[C:3]([O:14][C@H:15]2[CH2:19][NH:18][C@H:17]([C:27]([O:29][CH3:30])=[O:28])[CH2:16]2)=[N:4][C:5]2[C:10]([N:11]=1)=[CH:9][CH:8]=[C:7]([O:12][CH3:13])[CH:6]=2

参加物

5

反応物 3

HCID 313Hydrochloric Acid2 回HCID 312751,4-Dioxane2 回HCID 584284571-(tert-Butyl) 2-methyl (2S,4R)-4-((3-chloro-7-methoxyquinoxalin-2-yl)oxy)pyrrolidine-1,2-dicarboxylate

生成物 1

HCID 78358295Methyl (2S)-4-((3-chloro-7-methoxyquinoxalin-2-yl)oxy)pyrrolidine-2-carboxylate hydrochloride収率 95%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
20 °C

実験手順

A solution (0.62 M) of 1-tert-butyl 2-methyl (2S,4R)-4-[(3-chloro-7-methoxyquinoxalin-2-yl)oxy]pyrrolidine-1,2-dicarboxylate in CH2Cl2 was treated with a solution (4 M) of HCl in dioxane (5 eq). The mixture was stirred at 20° C. for 2 h, then treated with a solution (4 M) of HCl in dioxane (2 eq). After 5 h, the reaction was judged complete and the mixture was concentrated under reduced pressure. The residue was triturated with Et2O to give the title compound (95%) as a solid. MS (ES+) m/z 338 (M+H)+

後処理

  1. waitAfter 5 h
  2. concentrationthe mixture was concentrated under reduced pressure
  3. customThe residue was triturated with Et2O

出典と根拠

ORDレコード
ord-209cb44959954754a9acdb8ce4e119df
出典データセット
uspto-grants-2011_12
特許番号
US08080654B2

反応ノート

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