Hydrochloric Acid → 2-Methylthiophene-3-carboxylic acid

HRID 644802

反応式

HRID 644802 の反応式
[CH3:1][C:2]1[S:3][CH:4]=[CH:5][C:6]=1[C:7]([O:9]CC)=[O:8].[OH-].[Na+].Cl>C(O)C.O>[CH3:1][C:2]1[S:3][CH:4]=[CH:5][C:6]=1[C:7]([OH:9])=[O:8]

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 10464736Ethyl 2-methylthiophene-3-carboxylate

生成物 1

HCID 46254092-Methylthiophene-3-carboxylic acid収率 77%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

Ethyl 2-methyl-3-thiophenecarboxylate (3.42 g, 20.09 mmol; see step (ii) above) was dissolved in ethanol (5 mL) to which was added a solution of sodium hydroxide (3.2145 mg, 80.362 mmol) in water (10 mL). The reaction mixture was heated under reflux for 2 h. The volume was reduced to half under reduced pressure at 40° C. and the residue was cooled with ice water. Dilute HCl was added dropwise with stirring until pH 2. The white solid material was filtered off, washed with water and dried under reduced pressure at 50° C. to give the required material (2.1850 mg, 77% yield), m.p. 115-117° C., lit. m.p. 116-117° C. (see D. W. Knight, A. P. Nott J. Chem. Soc., Perkin Trans. 1 791-794 (1983)).

後処理

  1. temperatureThe reaction mixture was heated
  2. temperatureunder reflux for 2 h
  3. customwas reduced to half under reduced pressure at 40° C.
  4. filtrationThe white solid material was filtered off
  5. washwashed with water
  6. customdried under reduced pressure at 50° C.

出典と根拠

ORDレコード
ord-f49607a9e93249daaab070e2dcce2746
出典データセット
uspto-grants-2010_04
特許番号
US07700765B2

関連ノート

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