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N-[6-(Cyanomethyl)-3-pyridinyl]-4-(1-methylethyl)benzenesulfonamide → HCID 67420415, 화합물

HRID 1518197
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HRID 1518197 반응식
[C:1]([CH2:3][C:4]1[N:9]=[CH:8][C:7]([NH:10][S:11]([C:14]2[CH:19]=[CH:18][C:17]([CH:20]([CH3:22])[CH3:21])=[CH:16][CH:15]=2)(=[O:13])=[O:12])=[CH:6][CH:5]=1)#[N:2]>C(O)C.[Ni]>[NH2:2][CH2:1][CH2:3][C:4]1[N:9]=[CH:8][C:7]([NH:10][S:11]([C:14]2[CH:15]=[CH:16][C:17]([CH:20]([CH3:22])[CH3:21])=[CH:18][CH:19]=2)(=[O:13])=[O:12])=[CH:6][CH:5]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 67419651N-[6-(Cyanomethyl)-3-pyridinyl]-4-(1-methylethyl)benzenesulfonamide

생성물 1

HCID 67420415HCID 67420415, 화합물

시약·촉매·용매 2

HCID 935Nickel촉매HCID 702Ethanol용매

실험 절차

A mixture of N-(6-cyanomethyl-pyridin-3-yl)-4-isopropyl-benzenesulfonamide (1.7 g, 5.4 mmol) aqueous ammonia (45 ml) and raney-nickel (2.7 mmol) in ethanol (50 ml) was hydrogenated at atmospheric pressure. After filtration the mixture was concentrated under reduced pressure. The residue was partitioned between ethyl acetate and saturated aqueous NaHCO3 and the aqueous layer extracted five times with ethyl acetate. The combined organic layers were dried over MgSO4, filtered, and the solvent evaporated under reduced pressure to give the product as a yellow powder after recrystallisation from methanol/ethyl acetate (1.3 g, 73%).

후처리

  1. filtrationAfter filtration the mixture
  2. concentrationwas concentrated under reduced pressure
  3. customThe residue was partitioned between ethyl acetate and saturated aqueous NaHCO3
  4. extractionthe aqueous layer extracted five times with ethyl acetate
  5. dry with materialThe combined organic layers were dried over MgSO4
  6. filtrationfiltered
  7. customthe solvent evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-00fd3fb316d546b6aff95c6c290da6be
출처 데이터셋
uspto-grants-2012_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08232426B2

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