1,4-Dioxane hydrochloride → (S)-benzyl 2-(4-aminophenylcarbamoyl)pyrrolidine-1-carboxylate

HRID 44453

反応式

HRID 44453 の反応式
C(OC([NH:8][C:9]1[CH:14]=[CH:13][C:12]([NH:15][C:16]([C@@H:18]2[CH2:22][CH2:21][CH2:20][N:19]2[C:23]([O:25][CH2:26][C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)=[O:24])=[O:17])=[CH:11][CH:10]=1)=O)(C)(C)C.O1CCOCC1.Cl>O1CCOCC1>[NH2:8][C:9]1[CH:14]=[CH:13][C:12]([NH:15][C:16]([C@@H:18]2[CH2:22][CH2:21][CH2:20][N:19]2[C:23]([O:25][CH2:26][C:27]2[CH:28]=[CH:29][CH:30]=[CH:31][CH:32]=2)=[O:24])=[O:17])=[CH:11][CH:10]=1

参加物

4

反応物 2

HCID 204431481,4-Dioxane hydrochlorideHCID 59396122(S)-benzyl 2-(4-(tert-butoxycarbonylamino)phenylcarbamoyl)pyrrolidine-1-carboxylate

生成物 1

HCID 59396116(S)-benzyl 2-(4-aminophenylcarbamoyl)pyrrolidine-1-carboxylate収率 94.7%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

To a solution of the Product from Example 3A (0.245 g, 0.56 mmol) in dioxane (5 mL) was added 4M HCl dioxane (2.8 mL, 11.2 mol) and the mixture was stirred at ambient temperature for 17 hours. The mixture was concentrated and azeotroped with toluene to give a tan solid (0.18 g, 86%).

後処理

  1. concentrationThe mixture was concentrated
  2. customazeotroped with toluene

出典と根拠

ORDレコード
ord-2fb70fcb6ee44d94841669e1f407e784
出典データセット
uspto-grants-2013_09
特許番号
US08541424B2

関連ノート

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