HCID 20163820, compound → HCID 13765639, compound

HRID 256390Notes

Reaction equation

HRID 256390 reaction equation
[O:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[C:6]([O:8][CH:9]1[CH2:14][C:13]([CH3:16])([CH3:15])[NH:12][C:11]([CH3:18])([CH3:17])[CH2:10]1)=[O:7]>[Ni].CO>[O:1]1[CH2:5][CH2:4][CH2:3][CH:2]1[C:6]([O:8][CH:9]1[CH2:10][C:11]([CH3:18])([CH3:17])[NH:12][C:13]([CH3:16])([CH3:15])[CH2:14]1)=[O:7]

Participants

4

Reactant 1

HCID 20163820HCID 20163820, compound

Product 1

HCID 13765639HCID 13765639, compoundYield 75.5%

Reagents, catalysts & solvents 2

HCID 935NickelCatalystHCID 887MethanolSolvent

Procedure

15 g of 2,2,6,6-tetramethyl-4-piperidyl furan-2-carboxylate, 150 ml of methanol and 3 g of Raney nickel are introduced into a 0.3 l hydrogenation autoclave, and hydrogenation is carried out at 100° C. and under 100 bar until the pressure remains constant, which takes about 6 hours. The Raney nickel is filtered off, the filtrate is evaporated down and the residue is distilled under reduced pressure to give 11.5 g of a colorless oil of boiling point 118°-122° C./1.3 mbar.

Workup

  1. customis carried out at 100° C. and under 100 bar until the pressure
  2. filtrationThe Raney nickel is filtered off
  3. customthe filtrate is evaporated down
  4. distillationthe residue is distilled under reduced pressure

Sources & evidence

ORD record
ord-02218b6bd4a544d09f04bf3e680f44fd
Source dataset
uspto-grants-1987_10
Patent number
US04703072

Reaction notes

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