Water → HCID 10921471, compound
Reaction equation
[NH2:1][CH2:2][CH2:3][CH2:4][NH:5][CH2:6][CH2:7][NH:8][CH2:9][CH2:10][CH2:11][NH2:12].[CH:13]([CH:15]=O)=O.O>C1(C)C=CC=CC=1>[CH2:11]1[N:12]2[C@@H:7]([C@@H:6]3[N:1]([CH2:13][CH2:15]2)[CH2:2][CH2:3][CH2:4][NH:5]3)[NH:8][CH2:9][CH2:10]1Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Procedure
A solution of 87.2 g of 1,10-diamino-4,7-diazadecane in 500 ml of toluene was admixed with 72.3 g of a 40% aqueous glyoxal solution, and the mixture was refluxed, with a water separator fitted, for 3 hours. When the solution was cooled, a solid precipitated out which was filtered off with suction, washed three times with 50 ml of toluene each time and dried under reduced pressure. This gave 34.9 g of pale yellow needles.
Workup
- customseparator fitted, for 3 hours
- temperatureWhen the solution was cooled
- customa solid precipitated out which
- filtrationwas filtered off with suction
- washwashed three times with 50 ml of toluene each time
- customdried under reduced pressure
Sources & evidence
- ORD record
- ord-d0d3dd309a0348c2b14cb376eec42b1c
- Source dataset
- uspto-grants-2000_10
- Patent number
- US06130330
Reaction notes
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