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Water → 2-Oxo-4-trifluoromethyl-piperidine-1-carboxylic acid tert-butyl ester

HRID 1360163
ノート
印刷プレビュー

反応式

HRID 1360163 の反応式
[Na].[C:2]([O:6][C:7]([N:9]1[CH2:14][CH2:13][CH:12]([C:15]([F:18])([F:17])[F:16])[CH2:11][CH2:10]1)=[O:8])([CH3:5])([CH3:4])[CH3:3].[OH2:19]>C(OCC)(=O)C.[Ru]=O>[C:2]([O:6][C:7]([N:9]1[CH2:14][CH2:13][CH:12]([C:15]([F:18])([F:16])[F:17])[CH2:11][C:10]1=[O:19])=[O:8])([CH3:5])([CH3:3])[CH3:4]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 962WaterHCID 5360545SodiumHCID 49759149Tert-butyl 4-(trifluoromethyl)piperidine-1-carboxylate

生成物 1

HCID 669693432-Oxo-4-trifluoromethyl-piperidine-1-carboxylic acid tert-butyl ester収率 90%

試薬・触媒・溶媒 2

HCID 178527103HCID 178527103、化合物触媒
HCID 8857
Ethyl Acetate
溶媒
2 回

実験手順

2.82 g (3.2 mmol) of sodium methaperiodate (NaIO4) was dissolved in 20 mL of water, followed by addition of 117 mg (0.88 mmol) of ruthenium oxide (RuO2). To The reaction, was added a solution in which 660 mg (2.6 mmol) of 4-trifluoromethyl-piperidin-1-carboxylic acid t-butyl ester dissolved in 35 mL of ethyl acetate, followed by stirring for 2 hours and 20 minutes. The reaction solution was diluted with excess ethylacetate and washed once with water and aqueous NaCl, respectively, and then dried over anhydrous magnesium sulfate and filtered off. The filtrated solution was distilled off under reduced pressure, then the residue was purified by column chromatography (2:1 hexane:ethyl acetate) to give 0.63 g of the title compound in a yield of 90%.

後処理

  1. customTo The reaction
  2. washwashed once with water and aqueous NaCl
  3. dry with materialrespectively, and then dried over anhydrous magnesium sulfate
  4. filtrationfiltered off
  5. distillationThe filtrated solution was distilled off under reduced pressure
  6. customthe residue was purified by column chromatography (2:1 hexane:ethyl acetate)

出典と根拠

ORDレコード
ord-afe85805d0e34822b87683244d9466e8
出典データセット
uspto-grants-2011_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07879848B2

反応ノート

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