Water → Propylene glycol methyl ether acetate

HRID 716582Notes

Reaction equation

HRID 716582 reaction equation
[OH2:1].[O-:2][CH2:3][CH2:4]CC.[O-][CH2:8]CCC.[O-]CCCC.[O-]CCCC.[Ti+4:22].C[C:24]([OH:31])([CH2:28]CC)[CH2:25]CO>C(O)CCC>[CH3:28][CH:24]([O:31][C:3]([CH3:4])=[O:2])[CH2:25][O:1][CH3:8].[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, 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 [B-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, 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-78a90d4f490246df8a15edd79282e38a
Source dataset
uspto-grants-2015_11
Patent number
US09188866B2

Reaction notes

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