Trifluoroacetic acid → HCID 23136941、化合物
反応式
C(OC([N:8]1[CH2:12][CH2:11][CH:10]([N:13]([CH2:22][C:23](=[O:25])[NH2:24])[CH2:14][C:15]2[CH:20]=[CH:19][C:18]([Cl:21])=[CH:17][CH:16]=2)[CH2:9]1)=O)(C)(C)C.FC(F)(F)C(O)=O>ClCCl>[Cl:21][C:18]1[CH:19]=[CH:20][C:15]([CH2:14][N:13]([CH:10]2[CH2:11][CH2:12][NH:8][CH2:9]2)[CH2:22][C:23]([NH2:24])=[O:25])=[CH:16][CH:17]=1参加物
4
実験手順
A solution of 3-[carbamoylmethyl-(4-chloro-benzyl)-amino]-pyrrolidine-1-carboxylic acid tert-butyl ester (0.49 g, 1.32 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: 267 (M+1), UV retention time: 0.82 min.
後処理
- concentrationThe reaction mixture was concentrated in vacuo
- additiondiluted with ethyl acetate
- dry with materialThe combined organics were dried over sodium sulfate
- customThe product was used without any further purification ESI-MS m/z
出典と根拠
- ORDレコード
- ord-bdadf405822d42f8967d4cbce6434bfd
- 出典データセット
- uspto-grants-2014_02
- 特許番号
- US08653096B2
反応ノート
読み込み中…