Hydrochloric Acid → HCID 54338129, compound
Reaction equation
[CH2:1]([OH:5])[CH2:2][CH2:3][OH:4].[OH-].[K+].[CH2:8]=[CH:9][CH2:10][CH2:11]OS(C1C=CC(C)=CC=1)(=O)=O.Cl>O>[CH2:8]=[CH:9][CH2:10][CH2:11][O:4][CH2:3][CH2:2][CH2:1][OH:5]Participants
6
Reactant 4
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 75 °C
Procedure
Into a reactor, 1,3-propanediol (46.7 g) and potassium hydroxide (34.5 g) were charged and stirred, and heated at the internal temperature of 75° C. for 30 minutes. At the internal temperature of 80° C., CH2═CH(CH2)2OTs (69.5 g) obtained in EXAMPLE 3-1 was added thereto over 3 hours and standed as it is after stirring for 1 hour. The reaction mixture was poured into water (250 ml) and neutralized by adding hydrochloric acid. After filtration, the filtrate was extracted with t-butyl methyl ether (300 ml) four times. The organic layer put together was dried over magnesium sulfate and subjected to filtration, and the solvent was distilled off to obtain 5.5 g of CH2═CH(CH2)2O(CH2)3OH.
Workup
- stirringafter stirring for 1 hour
- filtrationAfter filtration
- extractionthe filtrate was extracted with t-butyl methyl ether (300 ml) four times
- dry with materialThe organic layer put together was dried over magnesium sulfate
- filtrationsubjected to filtration
- distillationthe solvent was distilled off
Sources & evidence
- ORD record
- ord-fb42bb7a19e440a895f9ce8b91c1f2c8
- Source dataset
- uspto-grants-2004_12
- Patent number
- US06833477B2
Reaction notes
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