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N-[6-(Cyanomethyl)-3-pyridinyl]-4-(1-methylethyl)benzenesulfonamide → HCID 67420415、化合物

HRID 1518197
ノート
印刷プレビュー

反応式

HRID 1518197 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

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

生成物 1

HCID 67420415HCID 67420415、化合物

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 702Ethanol溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-00fd3fb316d546b6aff95c6c290da6be
出典データセット
uspto-grants-2012_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08232426B2

反応ノート

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