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Methyl Salicylate → Methyl 2-(2,2,2-trifluoroethoxy)benzoate

HRID 1973185
ノート
印刷プレビュー

反応式

HRID 1973185 の反応式
[C:1]([O:10][CH3:11])(=[O:9])[C:2]1[C:3](=[CH:5][CH:6]=[CH:7][CH:8]=1)[OH:4].FC(F)(F)S(O[CH2:18][C:19]([F:22])([F:21])[F:20])(=O)=O.C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[F:20][C:19]([F:22])([F:21])[CH2:18][O:4][C:3]1[CH:5]=[CH:6][CH:7]=[CH:8][C:2]=1[C:1]([O:10][CH3:11])=[O:9]
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 4133Methyl SalicylateHCID 11430Potassium CarbonateHCID 803662,2,2-Trifluoroethyl trifluoromethanesulfonate

生成物 1

HCID 19622905Methyl 2-(2,2,2-trifluoroethoxy)benzoate

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

A mixture of methyl salicylate (6.4 ml., 7.6 g., 0.05 mole), 2,2,2-trifluoroethyl trifluoromethanesulfonate (13.9 g., 0.06 mole), anhydrous potassium carbonate (13.8 g., 0.1 mole) and acetone (150 ml.) is heated under reflux with efficient stirring for three days. The product is filtered and the filtrate is concentrated to a small volume. It is diluted with cold water and the resulting precipitate is collected and washed successively with cold dilute sodium hydroxide solution and water. The desired material is recrystallized then from aqueous ethanol to afford white solid, m.p. 61-62.

後処理

  1. temperatureis heated
  2. temperatureunder reflux
  3. filtrationThe product is filtered
  4. concentrationthe filtrate is concentrated to a small volume
  5. additionIt is diluted with cold water
  6. customthe resulting precipitate is collected
  7. washwashed successively with cold dilute sodium hydroxide solution and water
  8. customThe desired material is recrystallized
  9. customfrom aqueous ethanol to afford white solid, m.p. 61-62

出典と根拠

ORDレコード
ord-ce3af38a9ec54bc6bef429f0e4ade96f
出典データセット
uspto-grants-1976_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03996280

反応ノート

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