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

HRID 591086
ノート
印刷プレビュー

反応式

HRID 591086 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]>[Ni].O>[CH3:7][C:4]1([CH3:8])[CH:5]([OH:6])[C:2]([CH3:10])([CH3:1])[CH:3]1[OH:9]
参加物反応条件実験手順後処理出典と根拠反応ノート

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 935Nickel触媒HCID 962Water溶媒

反応条件

温度
100 °C

実験手順

A 300 mL Autoclave Engineers autoclave was charged with 25 grams of 2,2,4,4-tetramethylcyclobutane-1,3-dione, 87.50 grams Isopar™ G, 12.50 grams of water, and approximately 8 grams of washed raney nickel catalyst. 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 at approximately 1400 rpm and held for 5 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 97.3% selectivity to 2,2,4,4-tetramethycyclobutane-1,3-diol with a cis:trans ratio of 0.6:1.

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-05fb69ee03844ecd8795ae398833aefa
出典データセット
uspto-grants-2016_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09238603B1

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート