Butanal → 2-Propyl-1,3-dioxane

HRID 628928Notes

Reaction equation

HRID 628928 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 were carried out using the apparatus described above. Prior to each example, the column was heated to 100° C. with boiling water as described above. Butyraldehyde was fed through the bottom feed plate and a mixture of 1,3-propanediol and 500 ppmw phosphoric acid was fed through the upper feed plate at rates described in Table II. A butyraldehyde/water azeotrope was condensed overhead at 73° C. The basepot reached a maximum temperature of 165° C. Material was removed from the basepot throughout the run. The material separated into two phases, each of which was 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 was removed from the basepot throughout the run
  4. customThe material separated into two phases

Sources & evidence

ORD record
ord-e0b7be06a4da4f9fa669657fd48f9c2f
Source dataset
uspto-grants-2016_04
Patent number
US09315485B2

Reaction notes

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