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

HRID 591093

反応式

HRID 591093 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]>[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]

参加物

4

反応物 1

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 23950Ruthenium触媒HCID 3776Isopropanol溶媒

反応条件

温度
100 °C

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-377271b9f9174f0c93163bcf87f305b7
出典データセット
uspto-grants-2016_01
特許番号
US09238602B1

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