関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2,2,4,4-Tetramethyl-1,3-cyclobutanedione | HCID 13617 | — |
| 触媒 | Nickel | HCID 935 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2,2,4,4-Tetramethylcyclobutane-1,3-diol | HCID 76382 | — |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09238603B1 |
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| 出典データセット | uspto-grants-2016_01 |
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| ORD ID | ord-05fb69ee03844ecd8795ae398833aefa |
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| 出典メモ | uspto-grants-2016_01 |
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