Water → Propylene glycol methyl ether acetate

HRID 716581Notes

Reaction equation

HRID 716581 reaction equation
O.[CH3:2][CH:3]([CH3:5])[O-:4].[CH3:6][CH:7](C)[O-:8].C[CH:11](C)[O-:12].CC(C)[O-].[Ti+4:18].CC(O)(CC(O)C)C>CC(O)C>[CH3:2][CH:3]([O:4][C:7]([CH3:6])=[O:8])[CH2:5][O:12][CH3:11].[Ti:18]

Participants

6

Reactant 3

HCID 962WaterHCID 7870Hexylene GlycolHCID 11026Titanium isopropoxide

Product 2

HCID 7946Propylene glycol methyl ether acetateHCID 23963Titanium

Reagents, catalysts & solvents 1

HCID 3776IsopropanolSolvent2×

Procedure

IPA solution (500 g) of deionized water (27 g) was agitated with IPA solution (500 g) of a titanium tetraisopropoxide (284 g) and dropped at room temperature for 2 hours. 2-methyl-2,4-pentanediol (120 g) was added to a solution obtained and agitated at room temperature for 30 minutes. After the solution was concentrated under reduced pressure at 30° 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 40° C. until no BOH was distilled to obtain a PGMEA solution of a titanium-containing compound [B-II] (1,000 g) (compound concentration: 20%). The molecular weight (Mw) of the compound measured in terms of polystyrene was 1,100.

Workup

  1. additiondropped at room temperature for 2 hours
  2. customobtained
  3. concentrationAfter the solution was concentrated under reduced pressure at 30° C.
  4. temperatureit was heated to 60° C.
  5. temperatureheating
  6. additionThen, PGMEA (1,200 g) was added
  7. temperatureheated under reduced pressure at 40° C. until no BOH
  8. distillationwas distilled

Sources & evidence

ORD record
ord-c44b1f475ba843fa9fff59df7ef558d4
Source dataset
uspto-grants-2015_11
Patent number
US09188866B2

Reaction notes

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