Sodium borohydride → 4-Amino-6,6'-dimethyl-2,2'-bipyridine

HRID 1586928ノート

反応式

HRID 1586928 の反応式
[CH3:1][C:2]1[CH:3]=[C:4]([N+:16]([O-])=O)[CH:5]=[C:6]([C:9]2[CH:14]=[CH:13][CH:12]=[C:11]([CH3:15])[N:10]=2)[N+:7]=1[O-].[BH4-].[Na+]>CO.[Pd]>[NH2:16][C:4]1[CH:3]=[C:2]([CH3:1])[N:7]=[C:6]([C:9]2[CH:14]=[CH:13][CH:12]=[C:11]([CH3:15])[N:10]=2)[CH:5]=1

参加物

5

反応物 2

HCID 4311764Sodium borohydrideHCID 110321326,6'-Dimethyl-4-nitro-2,2'-bipyridine-N-oxide

生成物 1

HCID 197601464-Amino-6,6'-dimethyl-2,2'-bipyridine収率 80%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

6,6'-Dimethyl-4-nitro-2,2'-bipyridine-N-oxide (17) (2.0 g, 8.2 mmoles) was dissolved in methanol (20 ml). 10% palladium on carbon (0.36 g) was added followed by slow addition of sodium borohydride (3.6 g, 95 mmoles). After one hour the reaction mixture was filtered and the solution was evaporated. The residue was dissolved in 0.1N sodium hydroxide solution and the product was extracted with chloroform from the water phase. The chloroform phase was dried and evaporated. Yield: 80%

後処理

  1. filtrationAfter one hour the reaction mixture was filtered
  2. customthe solution was evaporated
  3. dissolutionThe residue was dissolved in 0.1N sodium hydroxide solution
  4. extractionthe product was extracted with chloroform from the water phase
  5. dry with materialThe chloroform phase was dried
  6. customevaporated

出典と根拠

ORDレコード
ord-4d57c6ee2b8449659bd38058f53038b3
出典データセット
uspto-grants-1993_06
特許番号
US05216134

反応ノート

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