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Methanol → Methyl 3-[(2S)-oxiran-2-yl]propanoate

HRID 2202241
ノート
印刷プレビュー

反応式

HRID 2202241 の反応式
[CH3:1][O-].[Na+].CO.CC1C=CC(S([O:16][CH2:17][C@@H:18]2[CH2:22][CH2:21][C:20](=[O:23])[O:19]2)(=O)=O)=CC=1.CO>C(O)(=O)C>[O:16]1[CH2:17][C@@H:18]1[CH2:22][CH2:21][C:20]([O:19][CH3:1])=[O:23]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 887MethanolHCID 2724793(S)-(5-Oxotetrahydrofuran-2-yl)methyl 4-methylbenzenesulfonateHCID 23694274Sodium methanolate methanol

生成物 1

HCID 10887939Methyl 3-[(2S)-oxiran-2-yl]propanoate収率 53%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

28% Sodium methoxide/MeOH solution (74.0 g, 383.35 mmol) was added to a mixture of (S)-(5-oxotetrahydrofuran-2-yl)methyl 4-methylbenzenesulfonate (51.81 g, 191.67 mmol) and dehydrated MeOH (280 mL) at room temperature, and the mixture was stirred at room temperature for 1.5 hr. The reaction mixture was cooled under ice-cooling, and the mixture was neutralized with acetic acid (about 15 mL). The reaction mixture was concentrated to about half-volume under reduced pressure, and ice water (350 mL) was added thereto. Then, the mixture was extracted with a mixed solvent of ethyl acetate/diethyl ether (3:1) (×3). The organic layer was washed successively with aqueous sodium hydrogencarbonate solution, water and brine, and dried over magnesium sulfate, and the solvent was evaporated under reduced pressure to give crude methyl (S)-3-(oxiran-2-yl)propanoate (13.12 g, 101 mmol, 53%) as a colorless oil.

後処理

  1. temperatureThe reaction mixture was cooled under ice-
  2. temperaturecooling
  3. concentrationThe reaction mixture was concentrated to about half-volume under reduced pressure, and ice water (350 mL)
  4. additionwas added
  5. extractionThen, the mixture was extracted with a mixed solvent of ethyl acetate/diethyl ether (3:1) (×3)
  6. washThe organic layer was washed successively with aqueous sodium hydrogencarbonate solution, water and brine
  7. dry with materialdried over magnesium sulfate
  8. customthe solvent was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-95ed873ca1ea4e34a1a32e282c31d6cd
出典データセット
uspto-grants-2016_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09365520B2

反応ノート

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