Hydrochloric Acid → HCID 54338129, compound

HRID 2308043Notes

Reaction equation

HRID 2308043 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

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

  1. stirringafter stirring for 1 hour
  2. filtrationAfter filtration
  3. extractionthe filtrate was extracted with t-butyl methyl ether (300 ml) four times
  4. dry with materialThe organic layer put together was dried over magnesium sulfate
  5. filtrationsubjected to filtration
  6. 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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