Sulfuric Acid → HCID 67486463、化合物

HRID 1511069ノート

反応式

HRID 1511069 の反応式
S(=O)(=O)(O)O.[CH3:6][C:7]1[C:8]([S:13][C:14]2[CH:15]=[C:16]([O:22][C:23]3[C:24]([CH3:29])=[N:25][CH:26]=[CH:27][CH:28]=3)[C:17]([C:20]#[N:21])=[N:18][CH:19]=2)=[N:9][CH:10]=[CH:11][CH:12]=1.[OH-:30].[Na+]>>[CH3:6][C:7]1[C:8]([S:13][C:14]2[CH:15]=[C:16]([O:22][C:23]3[C:24]([CH3:29])=[N:25][CH:26]=[CH:27][CH:28]=3)[C:17]([C:20]([NH2:21])=[O:30])=[N:18][CH:19]=2)=[N:9][CH:10]=[CH:11][CH:12]=1

参加物

4

反応物 3

HCID 1118Sulfuric AcidHCID 14798Sodium HydroxideHCID 67487618HCID 67487618、化合物

生成物 1

HCID 67486463HCID 67486463、化合物収率 94.9%

実験手順

Concentrated sulfuric acid (8 mL) was added to 5-(3-methylpyridin-2-ylthio)-3-(2-methylpyridin-3-yloxy)picolinonitrile (1.40 g, 4.19 mmol). The reaction was stirred over the weekend, then poured onto ice (100 g), cooled in an ice bath and made basic to pH 10 with 50% NaOH. The reaction mixture was extracted with ethyl acetate, washed with brine, dried (MgSO4), and concentrated to afford 5-(3-methylpyridin-2-ylthio)-3-(2-methylpyridin-3-yloxy)picolinamide (1.40 g, 3.97 mmol, 94.9% yield) as a colorless oil which became a white crystalline solid overnight under vacuo.

後処理

  1. additionpoured onto ice (100 g)
  2. temperaturecooled in an ice bath
  3. extractionThe reaction mixture was extracted with ethyl acetate
  4. washwashed with brine
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-9abbdec399c44f5db6df9cba022336c5
出典データセット
uspto-grants-2012_07
特許番号
US08212045B2

反応ノート

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