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Phosphoric Acid → HCID 57193292, 화합물

HRID 1050891
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HRID 1050891 반응식
CC(C)(CO)CO.[CH3:8][C:9]1([CH3:18])[CH2:14][O:13][CH:12]([CH2:15][CH2:16][CH3:17])[O:11][CH2:10]1.P(=O)(O)(O)O>[Pd].O>[CH2:12]([O:11][CH2:10][C:9]([CH3:8])([CH3:18])[CH2:14][OH:13])[CH2:15][CH2:16][CH3:17]
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참가 물질

6

반응물 3

HCID 1004Phosphoric AcidHCID 31344Neopentyl glycolHCID 2218875,5-Dimethyl-2-propyl-1,3-dioxane

생성물 1

HCID 57193292HCID 57193292, 화합물

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 962Water용매

반응 조건

온도
200 °C

실험 절차

90 g of 2,2-dimethyl-1,3-propanediol, 10 g of water, and 20 g of 5,5-dimethyl-2-propyl-1,3-dioxane were combined in a 300 mL autoclave with 1.5 g of 5% (by weight) Pd on carbon catalyst and 100 mg of phosphoric acid. The autoclave was sealed and purged twice with N2 and once with H2. The reactor was charged with H2 and heated to 200° C. The reactor was then brought to an operating pressure of 10.3 MPa and stirring commenced at 750 rpm. Pressure was maintained through the duration of the experiment. After 2 h, the autoclave was cooled and remaining gas vented. The autoclave was opened, its contents filtered, and the filtrate analyzed by gas chromatography (GC). 94% conversion of the acetal and 99% selectivity to 3-butoxy-2,2-dimethyl-propanol were observed.

후처리

  1. customThe autoclave was sealed
  2. custompurged twice with N2 and once with H2
  3. additionThe reactor was charged with H2
  4. temperaturePressure was maintained through the duration of the experiment
  5. temperaturethe autoclave was cooled
  6. filtrationits contents filtered

출처 및 근거

ORD 기록
ord-78ae6cd8bffd405bbbed130ac4a0e64a
출처 데이터셋
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09388105B2

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