Potassium Carbonate → 3-Hydroxy-2,2-dimethylpropyl 2,2,4-trimethyl-3-oxopentanoate

HRID 572710

反応式

HRID 572710 の反応式
[CH3:1][C:2]1([CH3:10])[C:5](=[O:6])[C:4]([CH3:8])([CH3:7])[C:3]1=[O:9].[OH:11][CH2:12][C:13]([CH3:17])([CH2:15]O)[CH3:14].C(=O)([O-])[O-:19].[K+].[K+]>C(Cl)Cl>[CH3:10][C:2]([CH3:1])([C:3](=[O:9])[CH:4]([CH3:7])[CH3:8])[C:5]([O:6][CH2:14][C:13]([CH3:17])([CH3:15])[CH2:12][OH:11])=[O:19]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 136172,2,4,4-Tetramethyl-1,3-cyclobutanedioneHCID 31344Neopentyl glycol

生成物 1

HCID 866671403-Hydroxy-2,2-dimethylpropyl 2,2,4-trimethyl-3-oxopentanoate収率 100%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a 1-liter round bottom flask was charged 2,2,4,4-tetramethyl-1,3-cyclobutanedione (140.2 g, 1.0 moles), neopentyl glycol (208.3 g, 2.0 moles), potassium carbonate (138 g, 1.0 moles) and 500 grams methylene chloride. The batch was heated to reflux for 3 hours then cooled and clarified to remove salts. Methylene chloride was removed with a rotary evaporator and 250 grams of toluene added. The organic layer was washed with 6×50 mL of demineralized water and dried with anhydrous sodium sulfate. Toluene was removed at 3 mmHg and 75° C. to provide 244.4 g of product. GC assay of the product was 96.2%.

後処理

  1. temperatureThe batch was heated
  2. temperatureto reflux for 3 hours
  3. temperaturethen cooled
  4. customto remove salts
  5. customMethylene chloride was removed with a rotary evaporator and 250 grams of toluene
  6. additionadded
  7. washThe organic layer was washed with 6×50 mL of demineralized water
  8. dry with materialdried with anhydrous sodium sulfate
  9. customToluene was removed at 3 mmHg and 75° C.

出典と根拠

ORDレコード
ord-5cca6038af9142acab008566e836fa34
出典データセット
uspto-grants-2015_05
特許番号
US09029451B2

関連ノート

読み込み中…