Tetrahydrofuran → HCID 12715767, 화합물

HRID 711708노트

반응식

HRID 711708 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-4642c5415b734e1987dfee4b9375683d
출처 데이터셋
uspto-grants-2015_11
특허 번호
US09181276B2

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