Tetrahydrofuran → HCID 12715767, 화합물

HRID 471571노트

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HRID 471571 반응식
[CH3:1][S:2][C:3]1[CH:10]=[CH:9][CH:8]=[C:7]([N+:11]([O-])=O)[C:4]=1[C:5]#[N:6].C1COCC1.CCOC(C)=O>CCO.[Pd]>[NH2:11][C:7]1[CH:8]=[CH:9][CH:10]=[C:3]([S:2][CH3:1])[C:4]=1[C:5]#[N:6]

참가 물질

6

반응물 3

HCID 8028TetrahydrofuranHCID 8857Ethyl AcetateHCID 12715768HCID 12715768, 화합물

생성물 1

HCID 12715767HCID 12715767, 화합물수율 79%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 702Ethanol용매

실험 절차

To a solution of 2-(methylthio)-6-nitrobenzonitrile (Example 104c) (1.5 g, 7.73 mmol) in EtOH (150 ml)/THF (50 ml)/EtOAc (50 ml) was added 200 mg of 10% Pd/C. The reaction mixture was hydrogenated on part shaker overnight. After the filtration, the filtered solution was dried down under vacuum, and the residue was purified by chromatography on silica gel eluting with EtOAc/Hexane to give the title compound (79%). 1H NMR (400 MHz, CDCl3) δ 2.51 (s, 3H), 4.47 (s, 2H), 6.53-6.51 (m, 1H), 6.58 (d, J=8.0 Hz, 1H), 7.27-7.21 (m, 1H).

후처리

  1. filtrationAfter the filtration
  2. customthe filtered solution was dried down under vacuum
  3. customthe residue was purified by chromatography on silica gel eluting with EtOAc/Hexane

출처 및 근거

ORD 기록
ord-11e73d900d8b40ac94751615a72b0f91
출처 데이터셋
uspto-grants-2014_01
특허 번호
US08633186B2

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