HCID 21252707, compound → HCID 21252704, compound

HRID 1530793Notes

Reaction equation

HRID 1530793 reaction equation
[F:1][C:2](=[C:6]1[CH2:15][CH2:14][C:9]2([O:13][CH2:12][CH2:11][O:10]2)[CH2:8][CH2:7]1)[CH:3]([F:5])[F:4].[H][H]>C(O)C.[Pd]>[F:1][CH:2]([CH:6]1[CH2:7][CH2:8][C:9]2([O:10][CH2:11][CH2:12][O:13]2)[CH2:14][CH2:15]1)[CH:3]([F:5])[F:4]

Participants

5

Reactant 2

HCID 21252707HCID 21252707, compoundHCID 178418361HCID 178418361, compound

Product 1

HCID 21252704HCID 21252704, compound

Reagents, catalysts & solvents 2

HCID 23938PalladiumCatalystHCID 702EthanolSolvent

Procedure

At atmospheric pressure, 22 g of 8-(1,2,2-trifluoroethylidene)-1,4-dioxaspiro[4.5]decane in 250 ml of ethanol in the presence of palladium on carbon as catalyst were hydrogenated until 2.2 liter of hydrogen had been taken up. The catalyst was subsequently filtered off and the filtrate was concentrated. The residue was chromatographed over silica gel (petroleum ether/ethyl acetate, 7:1), to give the title product as a colourless oil.

Workup

  1. filtrationThe catalyst was subsequently filtered off
  2. concentrationthe filtrate was concentrated
  3. customThe residue was chromatographed over silica gel (petroleum ether/ethyl acetate, 7:1)

Sources & evidence

ORD record
ord-490e7e46f6554abfbc73cd8b78ee0070
Source dataset
uspto-grants-2001_03
Patent number
US06197729B1

Reaction notes

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