Trifluoroacetic acid → HCID 65439120、化合物

HRID 2041894ノート

反応式

HRID 2041894 の反応式
[F:1][C:2]1[CH:3]=[C:4]([C:9]2([OH:20])[CH2:12][N:11](C(OC(C)(C)C)=O)[CH2:10]2)[CH:5]=[CH:6][C:7]=1[F:8].FC(F)(F)C(O)=O>ClCCl>[F:1][C:2]1[CH:3]=[C:4]([C:9]2([OH:20])[CH2:12][NH:11][CH2:10]2)[CH:5]=[CH:6][C:7]=1[F:8]

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 659188071,1-Dimethylethyl 3-(3,4-difluorophenyl)-3-hydroxy-1-azetidinecarboxylate

生成物 1

HCID 65439120HCID 65439120、化合物収率 75.5%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A mixture of tert-butyl 3-(3,4-difluorophenyl)-3-hydroxyazetidine-1-carboxylate (1.06 g, 3.72 mmol) and trifluoroacetic acid (3 ml) in dichloromethane (30 ml) was stirred at ambient temperature for 1.5 h. The solvent was evaporated and the crude product was purified on a Biotage Isolute SCX-3 SPE column (washed with methanol and eluted with methanol/triethylamine, 4:1) to give the title compound (0.52 g). MS m/z (rel. intensity, 70 eV) 185 (M+, 1), 156 (50), 141 (bp), 127 (58), 114 (90).

後処理

  1. customThe solvent was evaporated
  2. customthe crude product was purified on a Biotage Isolute SCX-3 SPE column (washed with methanol and eluted with methanol/triethylamine, 4:1)

出典と根拠

ORDレコード
ord-154574165eac406c87b3cc9c5dc9d2b6
出典データセット
uspto-grants-2013_11
特許番号
US08586572B2

反応ノート

読み込み中…