HCID 53751895, compound → HCID 19966406, compound

HRID 260265Notes

Reaction equation

HRID 260265 reaction equation
[C:1]1([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[CH:6]=[CH:5][C:4]([CH:7]=[CH:8][CH2:9][CH2:10][NH2:11])=[CH:3][CH:2]=1>[Pd].CO>[C:1]1([C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=2)[CH:2]=[CH:3][C:4]([CH2:7][CH2:8][CH2:9][CH2:10][NH2:11])=[CH:5][CH:6]=1

Participants

4

Reactant 1

HCID 53751895HCID 53751895, compound

Product 1

HCID 19966406HCID 19966406, compoundYield 88.3%

Reagents, catalysts & solvents 2

HCID 23938PalladiumCatalystHCID 887MethanolSolvent

Procedure

17 ml of methanol, 1.74 g of the product of Stage B and 0.17 g of 10% Pd on charcoal catalyst were placed in a hydrogenation apparatus and hydrogenation was maintained overnight. After filtering, washing and concentrating, the product was impasted in ethyl acetate, chilled, separated and dried under reduced pressure at 80° C. to obtain 1.55 g of the desired product melting at 260° C.

Workup

  1. temperaturewas maintained overnight
  2. filtrationAfter filtering
  3. washwashing
  4. concentrationconcentrating
  5. temperaturechilled
  6. customseparated
  7. customdried under reduced pressure at 80° C.

Sources & evidence

ORD record
ord-a97f1e5416314a74b09504ec85e0dccc
Source dataset
uspto-grants-1996_06
Patent number
US05527780

Reaction notes

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