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Trifluoroacetic acid → HCID 58778388、化合物

HRID 1372621
ノート
印刷プレビュー

反応式

HRID 1372621 の反応式
C(OC([N:8]1[CH2:12][C@@H:11]([F:13])[CH2:10][C@H:9]1[CH2:14][O:15][CH2:16][CH2:17][CH2:18][CH2:19][C:20]([O:22][CH3:23])=[O:21])=O)(C)(C)C.FC(F)(F)C(O)=O>C(Cl)Cl>[F:13][C@@H:11]1[CH2:12][NH:8][C@H:9]([CH2:14][O:15][CH2:16][CH2:17][CH2:18][CH2:19][C:20]([O:22][CH3:23])=[O:21])[CH2:10]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 67405510HCID 67405510、化合物

生成物 1

HCID 58778388HCID 58778388、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Methyl 5-((2S,4S)-1-(tert-butoxycarbonyl)-4-fluoro-2-pyrrolidinylmethoxy)pentanoate (1.09 g, 3.27 mmol) was dissolved in methylene chloride (50 ml). At room temperature, trifluoroacetic acid (10 ml) was added to the resulting solution. The mixture was stirred at the same temperature for 3.5 hours. The residue obtained by distilling off the solvent under reduced pressure was diluted with methylene chloride (50 ml). The solution was basified with 1N NaOH, followed by extraction with methylene chloride. The extract was washed with saturated brine, dried over anhydrous sodium sulfate and distilled under reduced pressure to remove the solvent, whereby the title compound (590 mg, 77%) was obtained as a yellow oil (this compound was provided for the subsequent reaction without further purification).

後処理

  1. customThe residue obtained
  2. distillationby distilling off the solvent under reduced pressure
  3. additionwas diluted with methylene chloride (50 ml)
  4. extractionfollowed by extraction with methylene chloride
  5. washThe extract was washed with saturated brine
  6. dry with materialdried over anhydrous sodium sulfate
  7. distillationdistilled under reduced pressure
  8. customto remove the solvent, whereby the title compound (590 mg, 77%)
  9. customwas obtained as a yellow oil (this compound
  10. customwas provided for the subsequent reaction without further purification)

出典と根拠

ORDレコード
ord-0808868cad7f4657904182285e2dd380
出典データセット
uspto-grants-2007_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07157487B2

反応ノート

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