Butanal → 2-Propyl-1,3-dioxane

HRID 73813Notes

Reaction equation

HRID 73813 reaction equation
[CH:1](=[O:5])[CH2:2][CH2:3][CH3:4].[CH2:6](O)[CH2:7][CH2:8][OH:9].P(=O)(O)(O)O.C(=O)CCC.O>O>[CH2:2]([CH:1]1[O:9][CH2:8][CH2:7][CH2:6][O:5]1)[CH2:3][CH3:4]

Participants

6

Reactant 4

HCID 261ButanalHCID 1004Phosphoric AcidHCID 104421,3-PropanediolHCID 86675365Butyraldehyde water

Product 1

HCID 2839812-Propyl-1,3-dioxane

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

Examples 5-7 are carried out using the apparatus described above. Prior to each example, the column is heated to 100° C. with boiling water as described above. Butyraldehyde is fed through the bottom feed plate and a mixture of 1,3-propanediol and 500 ppmw phosphoric acid is fed through the upper feed plate at rates described in Table I. A butyraldehyde/water azeotrope is condensed overhead at 73° C. The basepot reaches a maximum temperature of 165° C. Material is removed from the basepot throughout the run. The material separates into two phases, each of which is analyzed by gas chromatography. The results are listed in Table II.

Workup

  1. customcondensed overhead at 73° C
  2. customa maximum temperature of 165° C
  3. customMaterial is removed from the basepot throughout the run

Sources & evidence

ORD record
ord-f8a3daac2477484bad7123e64e1056c4
Source dataset
uspto-grants-2014_09
Patent number
US08829207B2

Reaction notes

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