Water → HCID 21474599、化合物

HRID 2294557ノート

反応式

HRID 2294557 の反応式
[H-].[Na+].[C:3]([C:6]1[CH:14]=[CH:13][C:9]([C:10]([OH:12])=[O:11])=[CH:8][CH:7]=1)(=[O:5])[CH3:4].[CH2:15](Br)[CH:16]=[CH2:17].O>CN(C=O)C>[C:3]([C:6]1[CH:14]=[CH:13][C:9]([C:10]([O:12][CH2:17][CH:16]=[CH2:15])=[O:11])=[CH:8][CH:7]=1)(=[O:5])[CH3:4]

参加物

6

反応物 4

HCID 962WaterHCID 7841Allyl bromideHCID 114704-Acetylbenzoic AcidHCID 24758Sodium hydride

生成物 1

HCID 21474599HCID 21474599、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

1.65 g (55 mmol) of sodium hydride (80% in oil) and 50 ml of DMF are introduced under a stream of nitrogen into a round-bottomed flask. 8.2 g (50 mmol) of 4-acetylbenzoic acid, dissolved in 100 ml of DMF, are added dropwise and the mixture is stirred at room temperature until gaseous evolution has ceased. 4.6 ml (55 mmol) of allyl bromide are then introduced and the mixture is stirred at room temperature for 24 hours. The reaction medium is poured into water, the mixture is extracted with ethyl ether and the organic phase is separated after settling has taken place, then dried over magnesium sulphate and evaporated. The residue obtained is purified by chromatography on a silica column, eluting with a mixture of dichloromethane and hexane (80:20). After evaporation of the solvents, 7.2 g (71%) of allyl ester are collected in the form of a colorless oil.

後処理

  1. additionare added dropwise
  2. stirringthe mixture is stirred at room temperature for 24 hours
  3. extractionthe mixture is extracted with ethyl ether
  4. customthe organic phase is separated after settling
  5. dry with materialdried over magnesium sulphate
  6. customevaporated
  7. customThe residue obtained
  8. customis purified by chromatography on a silica column
  9. washeluting with a mixture of dichloromethane and hexane (80:20)
  10. customAfter evaporation of the solvents, 7.2 g (71%) of allyl ester
  11. customare collected in the form of a colorless oil

出典と根拠

ORDレコード
ord-cf3c12404749401eac076227fa1f6924
出典データセット
uspto-grants-1997_11
特許番号
US05688817

反応ノート

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