HCID 13292769, compound → 77599-89-4

HRID 1382627Notes

Reaction equation

HRID 1382627 reaction equation
[N:1]([CH2:4][CH2:5][O:6][C:7]1[CH:12]=[CH:11][C:10](/[C:13](/[C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)=[C:14](\[C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)/[C:15]([F:18])([F:17])[F:16])=[CH:9][CH:8]=1)=[N+]=[N-]>CO.[Pd]>[NH2:1][CH2:4][CH2:5][O:6][C:7]1[CH:8]=[CH:9][C:10](/[C:13](/[C:25]2[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=2)=[C:14](\[C:19]2[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=2)/[C:15]([F:16])([F:17])[F:18])=[CH:11][CH:12]=1

Participants

4

Reactant 1

HCID 13292769HCID 13292769, compound

Product 1

HCID 1329277277599-89-4Yield 52.6%

Reagents, catalysts & solvents 2

HCID 23938PalladiumCatalystHCID 887MethanolSolvent

Procedure

7.40 g (18 mmoles) of (E)-1-[4-(2-azidoethoxy)-phenyl]-1,2-diphenyl-3,3,3-trifluoro-propene, prepared as described in Example 7, are dissolved in 100 ml of methanol, 0.70 g of a 5% palladium-on-carbon catalyst are added, and the mixture is hydrogenated for about one hour. The catalyst is filtered off, the solution is evaporated, and the residue is crystallized from hexane. 3.63 g (52.3%) of the aimed compound are obtained; m.p.: 71°-76° C.

Workup

  1. filtrationThe catalyst is filtered off
  2. customthe solution is evaporated
  3. customthe residue is crystallized from hexane

Sources & evidence

ORD record
ord-8acc8028724e4ab0a4db05f017fc0e64
Source dataset
uspto-grants-1989_02
Patent number
US04806685

Reaction notes

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