2,2,4,4-Tetramethyl-1,3-cyclobutanedione → 2,2,4,4-Tetramethylcyclobutane-1,3-diol

HRID 591093

반응식

HRID 591093 반응식
[CH3:1][C:2]1([CH3:10])[C:5](=[O:6])[C:4]([CH3:8])([CH3:7])[C:3]1=[O:9]>[Ru].C(O)(C)C>[CH3:7][C:4]1([CH3:8])[CH:5]([OH:6])[C:2]([CH3:10])([CH3:1])[CH:3]1[OH:9]

참가 물질

4

반응물 1

HCID 136172,2,4,4-Tetramethyl-1,3-cyclobutanedione

생성물 1

HCID 763822,2,4,4-Tetramethylcyclobutane-1,3-diol

시약·촉매·용매 2

HCID 23950Ruthenium촉매HCID 3776Isopropanol용매

반응 조건

온도
100 °C

실험 절차

A 2 liter Parr autoclave was charged with 100 grams of 2,2,4,4-tetramethylcyclobutane-1,3-dione, 300 grams of isopropyl alcohol, and 50 grams of 2% ruthenium on alumina (surface area=10 m2/g, purchased from BASF Catalysts). The autoclave was pressure purged three times with nitrogen and three times with hydrogen, and the pressure was increased to 3.5 MPa (500 psig) with hydrogen. The autoclave was heated to 100° C. with stirring and held for 6 hours at 3.5 MPa (500 psig). Analysis of the product by gas chromatography indicated that 99.8% conversion of the 2,2,4,4-tetramethylcyclobutane-1,3-dione was obtained with 99.9% selectivity to 2,2,4,4-tetramethycyclobutane-1,3-diol with a cis:trans ratio of 1.54:1.

후처리

  1. custompurged three times with nitrogen and three times with hydrogen
  2. temperaturethe pressure was increased to 3.5 MPa (500 psig) with hydrogen

출처 및 근거

ORD 기록
ord-377271b9f9174f0c93163bcf87f305b7
출처 데이터셋
uspto-grants-2016_01
특허 번호
US09238602B1

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