Water → Propylene glycol methyl ether acetate

HRID 708310Notes

Reaction equation

HRID 708310 reaction equation
[OH2:1].[O-:2][CH2:3][CH2:4][CH2:5]C.[O-:7][CH2:8][CH2:9]CC.[O-][CH2:13]CCC.[O-]CCCC.[Ti+4:22].CC(O)(CCC)CCO>C(O)CCC>[C:8]([O:7][CH:4]([CH3:5])[CH2:3][O:2][CH3:13])(=[O:1])[CH3:9].[Ti:22]

Participants

6

Reactant 3

HCID 962WaterHCID 21801Titanium tetrabutoxideHCID 223239593-Methylhexane-1,3-diol

Product 2

HCID 7946Propylene glycol methyl ether acetateHCID 23963Titanium

Reagents, catalysts & solvents 1

HCID 2631-ButanolSolvent2×

Procedure

1-butanol (BOH) solution (500 g) of deionized water (27 g) was agitated with BOH solution (500 g) of a titanium tetrabutoxide (340 g) and dropped at room temperature for 2 hours. 3-methyl-1,3-hexanediol (132 g) was added to a solution obtained and agitated at room temperature for 30 minutes. After the solution was concentrated under reduced pressure at 40° C., it was heated to 60° C. and heating was continued under reduced pressure to generate no distillate. Then, propylene glycol methyl ether acetate (PGMEA) (1,200 g) was added thereto and heated under reduced pressure at 50° C. until no BOH was distilled to obtain a PGMEA solution of a titanium-containing compound [A-III] (1,000 g) (compound concentration: 22%). The molecular weight (Mw) of the compound measured in terms of polystyrene was 1,250.

Workup

  1. additiondropped at room temperature for 2 hours
  2. customobtained
  3. concentrationAfter the solution was concentrated under reduced pressure at 40° C.
  4. temperatureit was heated to 60° C.
  5. temperatureheating
  6. additionThen, propylene glycol methyl ether acetate (PGMEA) (1,200 g) was added
  7. temperatureheated under reduced pressure at 50° C. until no BOH
  8. distillationwas distilled

Sources & evidence

ORD record
ord-bc6733e029984e77b79aa5e215db0b88
Source dataset
uspto-grants-2015_11
Patent number
US09176382B2

Reaction notes

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