Hydrochloric Acid → HCID 15137264、化合物

HRID 1741560ノート

反応式

HRID 1741560 の反応式
C[O:2][C:3]([C:5]1[CH:10]=[C:9]([C:11]2[CH:16]=[C:15]([C:17](OC)=[O:18])[N:14]=[C:13]([C:21](OC)=[O:22])[CH:12]=2)[CH:8]=[C:7]([C:25](OC)=[O:26])[N:6]=1)=O.[BH4-].[Na+].Cl>O1CCOCC1.O>[OH:18][CH2:17][C:15]1[CH:16]=[C:11]([C:9]2[CH:10]=[C:5]([CH2:3][OH:2])[N:6]=[C:7]([CH2:25][OH:26])[CH:8]=2)[CH:12]=[C:13]([CH2:21][OH:22])[N:14]=1

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 2762456Tetramethyl [4,4'-bipyridine]-2,2',6,6'-tetracarboxylateHCID 4311764Sodium borohydride

生成物 1

HCID 15137264HCID 15137264、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 312751,4-Dioxane溶媒

実験手順

50 g (128.77 mmol) of 2,2', 6,6'-tetra(methoxycarbonyl)-4,4'-bipyridine is dissolved in a mixture of 400 ml of dioxane/400 ml of water and, in portions, 48.71 g (1.28 mol) of sodium borohydride is added thereto. The mixture is stirred overnight at room temperature. The solution is acidified with 5N hydrochloric acid and evaporated to dryness. The residue is suspended in 1 liter of 1N sodium hydroxide solution and extracted three times with 250 ml of chloroform. The organic phases are dried over magnesium sulfate and evaporated under vacuum. The residue is recrystallized from ethanol/ether.

後処理

  1. additionis added
  2. customevaporated to dryness
  3. extractionextracted three times with 250 ml of chloroform
  4. dry with materialThe organic phases are dried over magnesium sulfate
  5. customevaporated under vacuum
  6. customThe residue is recrystallized from ethanol/ether

出典と根拠

ORDレコード
ord-8cb5219b9d394ea4b007966a524147c7
出典データセット
uspto-grants-1994_08
特許番号
US05334371

反応ノート

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