Water → HCID 14551712、化合物

HRID 265644ノート

反応式

HRID 265644 の反応式
[C:1]([CH:4]1[CH2:9][CH:8]([CH2:10][CH3:11])[O:7][C:5]1=[O:6])(=[O:3])[CH3:2].S(Cl)([Cl:15])(=O)=O.O>C1C=CC=CC=1>[Cl:15][C:4]1([C:1](=[O:3])[CH3:2])[CH2:9][CH:8]([CH2:10][CH3:11])[O:7][C:5]1=[O:6]

参加物

5

反応物 3

HCID 962WaterHCID 24648Sulfuryl chlorideHCID 110518973-Acetyl-5-Ethyldihydro-2(3H)-Furanone

生成物 1

HCID 14551712HCID 14551712、化合物

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

Into a solution of 58.2 g (0.37 moles) of α-acetyl-γ-ethyl-γ-butyrolactone [prepared according to J. Pharm. Sci. 52, 733 (1963)] in 60 cm3 benzene 50 g of (0.37 moles) of sulphuryl chloride are added dropwise under stirring and cooling in 2 hours, keeping the temperature of the reaction mixture between 5 and 10° C. After completing the addition the reaction mixture is let to warm to room temperature and stirred at this temperature until the gas formation ceases. Then it is poured into 400 cm3 of water, the phases are separated and the water is extracted with 200 cm3 of benzene. The benzene containing solution is washed with 100 cm3 of 5% sodium hydrogencarbonate solution. After evaporation the residual oil is distilled in vacuo. The title compound is obtained in the form of a colourless liquid in an amount of 58.9 g (82.5%), its boiling point is 91° C. at a pressure of 80 Pa, nD20 =1,4623.

後処理

  1. temperaturecooling in 2 hours
  2. customthe temperature of the reaction mixture between 5 and 10° C
  3. additionthe addition the reaction mixture
  4. stirringstirred at this temperature until the gas formation ceases
  5. customthe phases are separated
  6. extractionthe water is extracted with 200 cm3 of benzene
  7. washThe benzene containing solution is washed with 100 cm3 of 5% sodium hydrogencarbonate solution
  8. customAfter evaporation the residual oil
  9. distillationis distilled in vacuo

出典と根拠

ORDレコード
ord-f104a04c82b94b7fa0b1d74c0029ac95
出典データセット
uspto-grants-1997_07
特許番号
US05648498

反応ノート

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