Phosphoric Acid → 3-Methyl-2-butenal
Reaction equation
P(=O)(O)(O)O.[CH3:6][C:7](=[CH2:11])[CH2:8][CH:9]=[O:10]>>[CH3:11][C:7](=[CH2:6])[CH2:8][CH:9]=[O:10].[CH3:6][C:7]([CH3:11])=[CH:8][CH:9]=[O:10]Participants
4
Conditions
- Temperature
- 140 °C
Procedure
0.4 part of 75 percent strength aqueous phosphoric acid is added to 69.2 parts of 3-methyl-3-buten-1-al and the mixture is heated in a pressure vessel to 140° C. in the course of 5 minutes, whilst bringing the total pressure to 10 bars with nitrogen. After 70 minutes at the above temperature, the mixture is cooled to room temperature in the course of 5 minutes. After neutralizing the phosphoric acid, distillation at 100 mm Hg gives 4.2 parts of uncoverted 3-methyl-3-buten-1-al and 61.8 parts (95% of theory) of 3-methyl-2-buten-1-al of boiling point 77° C. This corresponds to a conversion of 94 percent.
Workup
- temperaturethe mixture is cooled to room temperature in the course of 5 minutes
- distillationthe phosphoric acid, distillation at 100 mm Hg
Sources & evidence
- ORD record
- ord-ef666b666cb04f089b877748ec6244c6
- Source dataset
- uspto-grants-1980_03
- Patent number
- US04192820
Reaction notes
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