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Methylamine → 2-Methylthiophene-3-carboxylic acid

HRID 1814503
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HRID 1814503 반응식
[Cl-].[CH3:2][C:3]1[S:4][CH:5]=[CH:6][C:7]=1[C:8]([O-:10])=[O:9].C1COCC1.CN>C(OCC)(=O)C>[CH3:2][C:3]1[S:4][CH:5]=[CH:6][C:7]=1[C:8]([OH:10])=[O:9]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6329MethylamineHCID 8028TetrahydrofuranHCID 225034702-Methyl-3-thiophenecarboxylate chloride

생성물 1

HCID 46254092-Methylthiophene-3-carboxylic acid수율 89.3%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

2-Methyl-3-thiophenecarboxylate chloride (60.5 g)/THF (300 ml) solution was added dropwise to a 40% aqueous solution of methylamine (400 ml) at 0° C. Ethyl acetate (2 l) was added thereto, and then the organic layer was washed sequentially with water, a 5N aqueous solution of hydrochloride acid, an aqueous solution of saturated of saturated sodium bicarbonate, water and brine, dried and evaporated. The resulting residue was crystallized from n-hexane, to give the title compound as a white powder (43.5 g, yield; 71.8%).

후처리

  1. washthe organic layer was washed sequentially with water
  2. dry with materiala 5N aqueous solution of hydrochloride acid, an aqueous solution of saturated of saturated sodium bicarbonate, water and brine, dried
  3. customevaporated
  4. customThe resulting residue was crystallized from n-hexane

출처 및 근거

ORD 기록
ord-543d502e31254f8e811ab60f5ce57690
출처 데이터셋
uspto-grants-2005_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06875761B2

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