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Acetic Acid → Methyl 3,3-dicyclohexyl-2-hydroxy-3-methoxypropionate

HRID 1584622
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HRID 1584622 반응식
[OH:1][CH:2]([C:7]([O:20][CH3:21])([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[C:3]([O:5][CH3:6])=[O:4].C(O)(=O)C>CO.O1CCOCC1>[CH:8]1([C:7]([CH:14]2[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]2)([O:20][CH3:21])[CH:2]([OH:1])[C:3]([O:5][CH3:6])=[O:4])[CH2:9][CH2:10][CH2:11][CH2:12][CH2:13]1
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참가 물질

5

반응물 2

HCID 176Acetic AcidHCID 10541193Methyl 2-hydroxy-3-methoxy-3,3-diphenylpropanoate

생성물 1

HCID 12073750Methyl 3,3-dicyclohexyl-2-hydroxy-3-methoxypropionate수율 97%

시약·촉매·용매 2

HCID 887Methanol용매HCID 312751,4-Dioxane용매

실험 절차

10 g (34.9 mmol) of methyl 2-hydroxy-3-methoxy-3,3-diphenylpropionate were dissolved in 50 ml each of methanol and glacial acetic acid, 1 ml of RuO(OH)2 in dioxane was added, and hydrogenation was carried out with H2 in an autoclave at 100° C. under 100 bar for 30 h. The catalyst was filtered off, the mixture was concentrated, mixed with ether and washed with NaCl solution, and the organic phase was dried and concentrated. 10.1 g of methyl 3,3-dicyclohexyl-2-hydroxy-3-methoxypropionate were obtained as an oil.

후처리

  1. filtrationThe catalyst was filtered off
  2. concentrationthe mixture was concentrated
  3. additionmixed with ether
  4. washwashed with NaCl solution
  5. customthe organic phase was dried
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-ebec55b6b58e441cbd918a6fac86e70e
출처 데이터셋
uspto-grants-1999_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05932730

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