Water → 1,4-Diethyl 2-formylbutanedioate

HRID 57787

反応式

HRID 57787 の反応式
[Na].[CH2:2]([O:4][C:5](=[O:13])[CH2:6][CH2:7][C:8]([O:10][CH2:11][CH3:12])=[O:9])[CH3:3].[CH2:14]([O:16]C=O)C.O>C(OCC)C>[CH2:2]([O:4][C:5](=[O:13])[CH:6]([CH:14]=[O:16])[CH2:7][C:8]([O:10][CH2:11][CH3:12])=[O:9])[CH3:3]

参加物

6

反応条件

温度
40 °C

実験手順

To a suspension of sodium (333 mg, 14 mmol, 1.2 eq) in diethyl ether (7 mL) were added succinic acid diethyl ester (2.1 g, 12 mmol, 1 eq) and formic acid ethyl ester (1.7 mL, 20 mmol, 1.7 eq). The mixture was stirred at 40° C. for 5 h. Water (10 mL) was added and the aqueous layer was washed with diethyl ether (2×10 mL). The aqueous layer was then acidified with a 6N solution of hydrochloric acid and extracted with diethyl ether (3×10 mL). The organic layers were dried over magnesium sulfate, filtered and evaporated in vacuo to afford the expected compound as orange oil (2.6 g, quant. yield).

後処理

  1. washthe aqueous layer was washed with diethyl ether (2×10 mL)
  2. extractionextracted with diethyl ether (3×10 mL)
  3. dry with materialThe organic layers were dried over magnesium sulfate
  4. filtrationfiltered
  5. customevaporated in vacuo

出典と根拠

ORDレコード
ord-2af018deacdc422e955be1e741a90177
出典データセット
uspto-grants-2016_09
特許番号
US09434745B2

関連ノート

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