Hydrochloric Acid → 2-Methylthiophene-3-carboxylic acid

HRID 644802

반응식

HRID 644802 반응식
[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]

참가 물질

6

반응물 3

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

생성물 1

HCID 46254092-Methylthiophene-3-carboxylic acid수율 77%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

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)).

후처리

  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.

출처 및 근거

ORD 기록
ord-f49607a9e93249daaab070e2dcce2746
출처 데이터셋
uspto-grants-2010_04
특허 번호
US07700765B2

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