Hydrochloric Acid → 3-Hydroxy-2-methoxy-1,2-diphenylpropan-1-one

HRID 851851

반응식

HRID 851851 반응식
[OH-:1].[K+].[CH3:3][O:4][CH:5]([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)[C:6](=[O:13])[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.[CH2:20]=O.Cl>C(O)C.O.CS(C)=O>[CH3:3][O:4][C:5]([CH2:20][OH:1])([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)[C:6](=[O:13])[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1

참가 물질

8

반응물 4

HCID 313Hydrochloric AcidHCID 712FormaldehydeHCID 14797Potassium HydroxideHCID 98097Methyl Benzoin

생성물 1

HCID 219095133-Hydroxy-2-methoxy-1,2-diphenylpropan-1-one

시약·촉매·용매 3

HCID 679Dimethyl Sulfoxide용매HCID 702Ethanol용매HCID 962Water용매

실험 절차

Potassium hydroxide 0.4 g was dissolved in ethanol 5 mL and dimethyl sulfoxide 200 mL was further added to obtain a solution. Benzoin methyl ether 30 g (0.13 mol) was dissolved in the solution and paraformaldehyde 5 g (0.16 mol) was added and reacted at 40° C. for 3 hours under nitrogen current. After that, the reaction product was cooled to a room temperature and neutralized with a dilute hydrochloric acid and then saturated salt water 120 mL was added. The solution was extracted by ethyl acetate and the extracted liquid was washed with saturated salt water three times. The washed product was dried and concentrated by anhydrous magnesium sulfate and recrystallized by diethyl ether. α-methylol benzoin methyl ether (MBME) was obtained in such a manner.

후처리

  1. customto obtain a solution
  2. additionwas added
  3. customreacted at 40° C. for 3 hours under nitrogen current
  4. extractionThe solution was extracted by ethyl acetate
  5. washthe extracted liquid was washed with saturated salt water three times
  6. customThe washed product was dried
  7. concentrationconcentrated by anhydrous magnesium sulfate
  8. customrecrystallized by diethyl ether

출처 및 근거

ORD 기록
ord-7a309612a73f478487bc80aaed6533eb
출처 데이터셋
uspto-grants-2007_08
특허 번호
US07253131B2

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