Carbon Dioxide → HCID 178513187, compound
Reaction equation
[C:1]1([PH:7](=[O:9])[OH:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C(=O)(O)O.[NH2:14][NH:15][C:16]([NH2:18])=[NH:17].C(=O)=O>>[C:1]1([PH:7](=[O:8])[OH:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[NH2:14][NH:15][C:16]([NH2:18])=[NH:17]Participants
4
Conditions
- Temperature
- 65 °C
Procedure
380.2 g (2.68 mol) phenylphosphinic acid (Aldrich, Germany) are dissolved at room temperature in 1.25 lethanol, and the solution is heated to 65° C. 364.2 g (2.68 mol) aminoguanidine hydrogencarbonate (Aldrich, Germany) is added over a period of 35 min. in small portions after each cessation of carbon dioxide evolution. After completing the addition, the mixture is stirred for another 90 min. at 65° C. The clear, colourless solution is concentrated to dryness in the rotary evaporator. The solid residue formed is dried at 60° C. over night in an air circulation drying oven and then for 17 h in a vacuum oven at 130° C. 578 g (2.68 mol, 99.8%) of the above product are obtained as a colourless, crystalline solid.
Workup
- additionthe addition
- concentrationThe clear, colourless solution is concentrated to dryness in the rotary evaporator
- customThe solid residue formed
- customis dried at 60° C. over night in an air circulation
- customdrying oven
- waitfor 17 h in a vacuum oven at 130° C
Sources & evidence
- ORD record
- ord-0be90cb4ec12438cbb738581a7a3c079
- Source dataset
- uspto-grants-2014_07
- Patent number
- US08771561B2
Reaction notes
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