Methanol → HCID 13523632、化合物

HRID 404997ノート

反応式

HRID 404997 の反応式
[CH2:1]([O:5][CH2:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)[C@H:2]1[O:4][CH2:3]1.[OH-:13].[K+].[CH3:15]O>>[CH2:6]([O:5][CH2:1][C@@H:2]([OH:4])[CH2:3][O:13][CH3:15])[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1

参加物

4

反応物 3

HCID 887MethanolHCID 14797Potassium HydroxideHCID 146296(+)-Benzyl glycidyl ether

生成物 1

HCID 13523632HCID 13523632、化合物収率 98%

反応条件

温度
30 °C

実験手順

To a stirred solution of (S)-benzyl glycidyl ether (S)-2 (4 g, 24.3 mmol) in methanol (40 mL) was added slowly a powdered KOH (4 g; 70 mmol) at 10° C. and the reaction mixture was stirred at 30° C. temperature for 8 h, after which the solvent was evaporated under reduced pressure. The residue was dissolved in ethylacetate (50 mL), washed with water, dried over Na2SO4, and evaporated under reduced pressure. The crude product was purified by column chromatography (silica gel, petroleum ether/acetone, 90:10) to afford (S)-1-(benzyloxy)-3-methoxypropan-2-ol (S)-3 as a colorless oil (4.6 g, 98%).

後処理

  1. customafter which the solvent was evaporated under reduced pressure
  2. dissolutionThe residue was dissolved in ethylacetate (50 mL)
  3. washwashed with water
  4. dry with materialdried over Na2SO4
  5. customevaporated under reduced pressure
  6. customThe crude product was purified by column chromatography (silica gel, petroleum ether/acetone, 90:10)

出典と根拠

ORDレコード
ord-a69777300fac424d92d4b661eeeee5c1
出典データセット
uspto-grants-2014_06
特許番号
US08748660B2

反応ノート

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