Hydrogen Peroxide → HCID 178510556, 화합물

HRID 240324노트

반응식

HRID 240324 반응식
[Cl:1][C:2]1[CH:18]=[CH:17][C:16]2[C:7]3=[N:8][C:9](C#N)=[C:10]([C:12]#[N:13])[N:11]=[C:6]3[C:5](=[O:19])[C:4]=2[CH:3]=1.[OH:20]O.ClCCl>CS(C)=O>[Cl:1][C:2]1[CH:18]=[CH:17][C:16]2[C:7]3=[N:8][C:9]([OH:20])=[C:10]([C:12]#[N:13])[N:11]=[C:6]3[C:5](=[O:19])[C:4]=2[CH:3]=1

참가 물질

5

반응물 3

HCID 784Hydrogen PeroxideHCID 6344DichloromethaneHCID 160657737-Chloro-9-oxo-9H-indeno[1,2-b]pyrazine-2,3-dicarbonitrile

생성물 1

HCID 178510556HCID 178510556, 화합물수율 70%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

To a suspension of 50 mg (0.19 mmol) 17g and 2.2 mg (5 Mol-%) Na2MoO4 in 2 ml DMSO was added dropwise 82 μl (0.95 mmol) of an aqueous solution of H2O2 (35%). The colour turned to red, and the mixture was stirred for 48 h at room temperature. After addition of 20 mL Dichloromethane, the resulting solution was washed with water and sat. brine (3×5 ml). After drying, filtration and evaporation, the crude product was purified by chromatography (DCM/MeOH 8/2) to yield 35 mg (70%) compound 42 as yellow-orange powder. 1H-NMR (d6-DMSO, 300 MHz): δ (ppm)=7.55 (s, 1H); 7.64 (m, 2H). ESI−MS: calcd for C12H4ClN3O2: 257.64; found: 255.9 (M-H+).

후처리

  1. washthe resulting solution was washed with water and sat. brine (3×5 ml)
  2. customAfter drying
  3. filtrationfiltration and evaporation
  4. customthe crude product was purified by chromatography (DCM/MeOH 8/2)

출처 및 근거

ORD 기록
ord-599a26d4bc2146bc92c298229b2262c1
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08648076B2

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