Trifluoroacetic acid → 2-[(4-Chloro-benzyl)-pyrrolidin-3-yl-amino]ethanol

HRID 242683ノート

反応式

HRID 242683 の反応式
C(OC([N:8]1[CH2:12][CH2:11][CH:10]([N:13]([CH2:17][C:18]2[CH:23]=[CH:22][C:21]([Cl:24])=[CH:20][CH:19]=2)[CH2:14][CH2:15][OH:16])[CH2:9]1)=O)(C)(C)C.FC(F)(F)C(O)=O>ClCCl>[Cl:24][C:21]1[CH:20]=[CH:19][C:18]([CH2:17][N:13]([CH:10]2[CH2:11][CH2:12][NH:8][CH2:9]2)[CH2:14][CH2:15][OH:16])=[CH:23][CH:22]=1

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 667586553-[(4-Chloro-benzyl)-(2-hydroxy-ethyl)-amino]-pyrrolidine-1-carboxylic acid tert-butyl ester

生成物 1

HCID 231368872-[(4-Chloro-benzyl)-pyrrolidin-3-yl-amino]ethanol

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A solution of 3-[(4-chloro-benzyl)-(2-hydroxy-ethyl)-amino]-pyrrolidine-1-carboxylic acid tert-butyl ester (0.22 g, 0.6 mmol) in dichloromethane cooled at 0° C. was treated with trifluoroacetic acid (20%). The resulting mixture was warmed to room temperature and stirred for 2 h. The reaction mixture was concentrated in vacuo, diluted with ethyl acetate and free based with 10% aqueous sodium bicarbonate. The combined organics were dried over sodium sulfate. The product was used without any further purification. ESI-MS m/z:255 (M+1), UV retention time: 0.34 min.

後処理

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. additiondiluted with ethyl acetate
  3. dry with materialThe combined organics were dried over sodium sulfate
  4. customThe product was used without any further purification

出典と根拠

ORDレコード
ord-5ba7a3dd8f764449af40040a3e667675
出典データセット
uspto-grants-2014_02
特許番号
US08653096B2

反応ノート

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