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5-Methanesulfonyl-furan-2-carboxylic acid methoxy-methyl-amide → 1-(5-Methanesulfonyl-furan-2-yl)-propan-1-one

HRID 1361166
ノート
印刷プレビュー

反応式

HRID 1361166 の反応式
CON(C)[C:4]([C:6]1[O:7][C:8]([S:11]([CH3:14])(=[O:13])=[O:12])=[CH:9][CH:10]=1)=[O:5].[CH2:16]([Mg]Cl)[CH3:17]>C1COCC1>[CH3:14][S:11]([C:8]1[O:7][C:6]([C:4](=[O:5])[CH2:16][CH3:17])=[CH:10][CH:9]=1)(=[O:12])=[O:13]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 592784855-Methanesulfonyl-furan-2-carboxylic acid methoxy-methyl-amideHCID 178461633HCID 178461633、化合物

生成物 1

HCID 592781411-(5-Methanesulfonyl-furan-2-yl)-propan-1-one

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a chilled (0° C.) solution of 5-methanesulfonyl-furan-2-carboxylic acid methoxy-methyl-amide (1.48 g, 6.36 mmol) in THF (30 mL) was added a 2 M solution of ethylmagnesium chloride in THF (7.0 mL, 14 mmol). The mixture was then slowly warmed to with stirring. After 18 hours, the mixture was quenched with saturated aqueous ammonium chloride (50 mL) and then diluted with ethyl acetate (50 mL). The aqueous phase was separated and extracted with ethyl acetate (3×30 mL). The combined organic layers were dried over sodium sulfate, filtered and concentrated to afford 1-(5-methanesulfonyl-furan-2-yl)-propan-1-one.

後処理

  1. temperatureThe mixture was then slowly warmed
  2. customthe mixture was quenched with saturated aqueous ammonium chloride (50 mL)
  3. additiondiluted with ethyl acetate (50 mL)
  4. customThe aqueous phase was separated
  5. extractionextracted with ethyl acetate (3×30 mL)
  6. dry with materialThe combined organic layers were dried over sodium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated

出典と根拠

ORDレコード
ord-6ea0f09aa53845f0bea7afba976b5c29
出典データセット
uspto-grants-2011_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07879873B2

反応ノート

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