Ethylene Glycol → 2-Hydroxyethyl 2,2,4-trimethyl-3-oxopentanoate

HRID 572709

반응식

HRID 572709 반응식
[CH2:1]([OH:4])[CH2:2][OH:3].[CH3:5][C:6]1([CH3:14])[C:9](=[O:10])[C:8]([CH3:12])([CH3:11])[C:7]1=[O:13].C(=O)([O-])[O-].[K+].[K+]>O>[CH3:11][C:8]([CH3:12])([C:9](=[O:10])[CH:6]([CH3:14])[CH3:5])[C:7]([O:3][CH2:2][CH2:1][OH:4])=[O:13]

참가 물질

5

반응물 3

HCID 174Ethylene GlycolHCID 11430Potassium CarbonateHCID 136172,2,4,4-Tetramethyl-1,3-cyclobutanedione

생성물 1

HCID 5183742-Hydroxyethyl 2,2,4-trimethyl-3-oxopentanoate

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a 2-liter round bottom flask was charged ethylene glycol (800 mL) and 2,2,4,4-tetramethyl-1,3-cyclobutanedione (185.8 g, 1.33 moles). While using good mixing, potassium carbonate (91.4 grams, 0.663 moles) was added. An exothermic reaction resulted and the batch temperature rose to approximately 65° C. The reaction was held for 1 hour between 50-60° C. The batch was then drowned into 1300 mL demineralized water and extracted with 800 mL ethyl acetate. The ethyl acetate layer was washed several times with water and dried with anhydrous sodium sulfate. The ethyl acetate was removed at 75° C. under 5 mmHg vacuum and the resulting crude product distilled through a 0.5×6 inch Penn-State packed column to provide 153 g of distilled product. The vapor boiling point was recorded as 113° C. at a pot temperature of 135° C. at <1 mmHg vacuum. The GC assay of the resulting product was 97.2%.

후처리

  1. additionwas added
  2. customAn exothermic reaction
  3. customresulted
  4. customrose to approximately 65° C
  5. extractionextracted with 800 mL ethyl acetate
  6. washThe ethyl acetate layer was washed several times with water
  7. dry with materialdried with anhydrous sodium sulfate
  8. customThe ethyl acetate was removed at 75° C. under 5 mmHg vacuum
  9. distillationthe resulting crude product distilled through a 0.5×6 inch Penn-State

출처 및 근거

ORD 기록
ord-3084b49a4dfa4335827360ee52c80fbe
출처 데이터셋
uspto-grants-2015_05
특허 번호
US09029451B2

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