Ethanol → Ethyl 5-chloro-2-methylbenzoate

HRID 1269518ノート

反応式

HRID 1269518 の反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([CH3:11])=[C:6]([CH:10]=1)[C:7]([OH:9])=[O:8].S(=O)(=O)(O)O.[CH2:17](O)[CH3:18]>>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([CH3:11])=[C:6]([CH:10]=1)[C:7]([O:9][CH2:17][CH3:18])=[O:8]

参加物

4

反応物 3

HCID 702EthanolHCID 1118Sulfuric AcidHCID 820095-Chloro-2-methylbenzoic acid

生成物 1

HCID 21269135Ethyl 5-chloro-2-methylbenzoate

実験手順

5-chloro-2-methylbenzoic acid (5.04 g, 29.5 mmol) was dissolved in 100 mL ethanol in a 250 mL round bottom flask fitted with a water condenser. 0.5 mL concentrated sulfuric acid was added and the solution heated to reflux. The solution was heated for 48 h and cooled to ambient temperature. The ethanol was removed under reduced pressure. The resultant oil was taken up in 300 mL diethyl ether and washed with saturated aqueous sodium bicarbonate (2×300 mL). The organic layer was dried over Na2SO4, filtered and concentrated under reduced pressure to yield 5.12 (87%) of ethyl 5-chloro-2-methylbenzoate as a clear oil.

後処理

  1. customfitted with a water condenser
  2. temperaturethe solution heated to reflux
  3. temperatureThe solution was heated for 48 h
  4. customThe ethanol was removed under reduced pressure
  5. washwashed with saturated aqueous sodium bicarbonate (2×300 mL)
  6. dry with materialThe organic layer was dried over Na2SO4
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-c1b94d6512874838a504e3655f49e08a
出典データセット
uspto-grants-2007_04
特許番号
US07199243B2

反応ノート

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