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

HRID 591095

반응식

HRID 591095 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
80 °C

실험 절차

A 2 liter Parr autoclave was charged with 100 grams of 2,2,4,4-tetramethylcyclobutane-1,3-dione, 300 grams Isopar™ G, 100 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 80° C. with stirring at approximately 1400 rpm and held for 6 hours at 3.5 MPa (500 psig). Analysis of the product by gas chromatography indicated that complete conversion of the 2,2,4,4-tetramethylcyclobutane-1,3-dione was obtained with 100% selectivity to 2,2,4,4-tetramethycyclobutane-1,3-diol with a cis:trans ratio of 1.44:1.

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-b636e14dc4be49e2850fafc5baa1c913
출처 데이터셋
uspto-grants-2016_01
특허 번호
US09238602B1

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