Methyl 5-((hydroxyimino)methyl)thiophene-2-carboxylate → HCID 14871948, 화합물

HRID 1397239

반응식

HRID 1397239 반응식
O[N:2]=[CH:3][C:4]1[S:8][C:7]([C:9]([O:11][CH3:12])=[O:10])=[CH:6][CH:5]=1>C(OC(=O)C)(=O)C>[C:3]([C:4]1[S:8][C:7]([C:9]([O:11][CH3:12])=[O:10])=[CH:6][CH:5]=1)#[N:2]

참가 물질

3

반응물 1

HCID 72740488Methyl 5-((hydroxyimino)methyl)thiophene-2-carboxylate

생성물 1

HCID 14871948HCID 14871948, 화합물수율 99.7%

시약·촉매·용매 1

HCID 7918Acetic Anhydride용매

실험 절차

A solution of methyl 5-((hydroxyimino)methyl)thiophene-2-carboxylate (440 mg, 2.4 mmol) in acetic anhydride (10 mL) was refluxed for 16 h. After completion, the reaction mixture was cooled to room temperature, concentrated under reduced pressure and the residue was dissolved in diethyl ether. The organic layer was washed with 10% aqueous NaOH solution, water and brine, and dried over anhydrous sodium sulfate. The solvent was removed under reduced pressure to yield methyl 5-cyanothiophene-2-carboxylate (5-cyano-thiophene-2-carboxylic acid methyl ester) (400 mg, yield 90%) which was carried through without any further purification. 1H NMR (400 MHz, DMSO-d6) δ 7.77 (d, J=4.2 Hz, 1H), 7.60 (d, J=4.1 Hz, 1H), 3.95 (s, 3H).

후처리

  1. concentrationconcentrated under reduced pressure
  2. dissolutionthe residue was dissolved in diethyl ether
  3. washThe organic layer was washed with 10% aqueous NaOH solution, water and brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. customThe solvent was removed under reduced pressure

출처 및 근거

ORD 기록
ord-a5fb5d6652714366a689781b8c78d6d9
출처 데이터셋
uspto-grants-2014_12
특허 번호
US08901156B2

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