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Dimethylformamide → HCID 89854217, 화합물

HRID 931127
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HRID 931127 반응식
Br[C:2]1[CH:3]=[C:4]([S:8]([NH:11][CH3:12])(=[O:10])=[O:9])[CH:5]=[N:6][CH:7]=1.[CH3:13][N:14](C)C=O>[C-]#N.[Zn+2].[C-]#N>[C:13]([C:2]1[CH:3]=[C:4]([S:8]([NH:11][CH3:12])(=[O:10])=[O:9])[CH:5]=[N:6][CH:7]=1)#[N:14]
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4

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HCID 6228DimethylformamideHCID 467389795-Bromo-N-methylpyridine-3-sulfonamide

생성물 1

HCID 89854217HCID 89854217, 화합물

시약·촉매·용매 1

HCID 11186Zinc cyanide (Zn(CN)2)촉매

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온도
100 °C

실험 절차

To a solution of 5-bromo-N-methylpyridine-3-sulfonamide (0.1 g, 0.39 mmol) in N,N-dimethylformamide was added zinc cyanide (0.056 g, 0.47 mmol). The solution was degassed with nitrogen for 10 min, then tetrakis(triphenylphosphine)palladium(0) (30 mg) was added. The reaction mixture was heated to 100° C. for 2 h. The mixture was then diluted with water and extracted with ethyl acetate. The organic layer was dried, filtered, and concentrated under reduced pressure. The crude compound was purified by rinsing with diethyl ether to afford 5-cyano-N-methylpyridine-3-sulfonamide (60 mg) which was used without further purification.

후처리

  1. customThe solution was degassed with nitrogen for 10 min
  2. additiontetrakis(triphenylphosphine)palladium(0) (30 mg) was added
  3. additionThe mixture was then diluted with water
  4. extractionextracted with ethyl acetate
  5. customThe organic layer was dried
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure
  8. customThe crude compound was purified
  9. washby rinsing with diethyl ether

출처 및 근거

ORD 기록
ord-9f254e608b4342e2ab6a2f1954aaf2cc
출처 데이터셋
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09296745B2

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