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Methylamine → n-Methyl-2-methylthiophene-3-carboxamide

HRID 1251185
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HRID 1251185 반응식
[Cl-].[CH3:2][C:3]1[S:4][CH:5]=[CH:6][C:7]=1[C:8]([O-:10])=O.C1COCC1.[CH3:16][NH2:17]>C(OCC)(=O)C>[CH3:16][NH:17][C:8]([C:7]1[CH:6]=[CH:5][S:4][C:3]=1[CH3:2])=[O:10]
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참가 물질

5

반응물 3

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

생성물 1

HCID 22503091n-Methyl-2-methylthiophene-3-carboxamide수율 71.8%

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 hydrochloric acid, an aqueous solution 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 hydrochloric acid, an aqueous solution 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-6da2f436209b4808827cb0ddcc1ec0f5
출처 데이터셋
uspto-grants-2002_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06340759B1

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