HCID 67406569、化合物 → HCID 67406325、化合物

HRID 1372625ノート

反応式

HRID 1372625 の反応式
C([O:8][CH2:9]/[CH:10]=[CH:11]\[CH2:12][O:13][CH2:14][C@@H:15]1[CH2:19][C@H:18]([F:20])[CH2:17][N:16]1[C:21]([O:23][C:24]([CH3:27])([CH3:26])[CH3:25])=[O:22])C1C=CC=CC=1>C(O)C.[OH-].[Pd+2].[OH-]>[C:24]([O:23][C:21]([N:16]1[CH2:17][C@@H:18]([F:20])[CH2:19][C@H:15]1[CH2:14][O:13][CH2:12][CH2:11][CH2:10][CH2:9][OH:8])=[O:22])([CH3:27])([CH3:26])[CH3:25]

参加物

4

反応物 1

HCID 67406569HCID 67406569、化合物

生成物 1

HCID 67406325HCID 67406325、化合物収率 68.6%

試薬・触媒・溶媒 2

HCID 9942167Palladium hydroxide触媒HCID 702Ethanol溶媒

実験手順

In ethanol (200 ml) were suspended (Z)-(2S,4S)-2-(4-benzyloxy-2-butenyloxymethyl)-1-(tert-butoxycarbonyl)-4-fluoropyrrolidine (4.58 g, 12.1 mmol) and 20% palladium hydroxide (4.0 g). The resulting suspension was subjected to catalytic hydrogenation at room temperature under normal pressure for 14 hours. The catalyst was then filtered off and the filtrate was distilled under reduced pressure to remove the solvent. The residue was purified by chromatography on a silica gel column (silica gel: 100 g), whereby from chloroform/acetone (10/1) eluate fractions, the title compound (2.42 g, 67%) was obtained as a colorless oil.

後処理

  1. filtrationThe catalyst was then filtered off
  2. distillationthe filtrate was distilled under reduced pressure
  3. customto remove the solvent
  4. customThe residue was purified by chromatography on a silica gel column (silica gel: 100 g), whereby from chloroform/acetone (10/1) eluate fractions

出典と根拠

ORDレコード
ord-1241dc4f90d44816bd17b9d4d852b94a
出典データセット
uspto-grants-2007_01
特許番号
US07157487B2

反応ノート

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