Trifluoroacetic acid → HCID 23136941、化合物

HRID 557067ノート

反応式

HRID 557067 の反応式
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

反応物 2

HCID 6422Trifluoroacetic acidHCID 66758387HCID 66758387、化合物

生成物 1

HCID 23136941HCID 23136941、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

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

  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 ESI-MS m/z

出典と根拠

ORDレコード
ord-85672b43c64c4ba889fca866ddd84e92
出典データセット
uspto-grants-2011_11
特許番号
US08058287B2

反応ノート

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