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

HRID 851851

反応式

HRID 851851 の反応式
[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

参加物

8

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 3

HCID 679Dimethyl Sulfoxide溶媒HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-7a309612a73f478487bc80aaed6533eb
出典データセット
uspto-grants-2007_08
特許番号
US07253131B2

関連ノート

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