HCID 12403260, compound → HCID 11552324, compound

HRID 658325Notes

Reaction equation

HRID 658325 reaction equation
[C:1]([CH2:3][CH2:4][N:5]([CH2:10][C:11]1[CH:16]=[CH:15][CH:14]=[C:13]([CH2:17][N:18]([CH2:23][CH2:24][C:25]#[N:26])[CH2:19][CH2:20][C:21]#[N:22])[CH:12]=1)[CH2:6][CH2:7][C:8]#[N:9])#[N:2].[H][H]>O1CCOCC1>[NH2:22][CH2:21][CH2:20][CH2:19][N:18]([CH2:17][C:13]1[CH:14]=[CH:15][CH:16]=[C:11]([CH2:10][N:5]([CH2:4][CH2:3][CH2:1][NH2:2])[CH2:6][CH2:7][CH2:8][NH2:9])[CH:12]=1)[CH2:23][CH2:24][CH2:25][NH2:26]

Participants

4

Reactant 2

HCID 12403260HCID 12403260, compoundHCID 178418361HCID 178418361, compound

Product 1

HCID 11552324HCID 11552324, compoundYield 94.3%

Reagents, catalysts & solvents 1

HCID 312751,4-DioxaneSolvent

Procedure

6.97 g of 1,3-bis(N,N-bis(2-cyanoethyl)aminomethyl)benzene, 0.70 g of Raney Co and 100 mL of 1,4-dioxane were charged in an autoclave and a hydrogenation reaction was carried out at an initial hydrogen pressure of 9.0 MPa at 180° C. for 2 hours. After the catalyst was removed by filtration, the obtained filtrate was concentrated to dryness to give 6.88 g of the title compound.

Workup

  1. customa hydrogenation reaction
  2. customAfter the catalyst was removed by filtration
  3. concentrationthe obtained filtrate was concentrated to dryness

Sources & evidence

ORD record
ord-24f8ab61f7e74a02a8337cb599a0c5ab
Source dataset
uspto-grants-2011_12
Patent number
US08076478B2

Reaction notes

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