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

HRID 591086

반응식

HRID 591086 반응식
[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]

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 935Nickel촉매HCID 962Water용매

반응 조건

온도
100 °C

실험 절차

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.

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-05fb69ee03844ecd8795ae398833aefa
출처 데이터셋
uspto-grants-2016_01
특허 번호
US09238603B1

연결된 노트

불러오는 중…