Water → 4-(Hydroxymethyl)pyridine-2-carboxamide

HRID 493233ノート

反応式

HRID 493233 の反応式
C[Si](Cl)(C)C.[C:6]([C:8]1[CH:13]=[C:12]([CH2:14][OH:15])[CH:11]=[CH:10][N:9]=1)#[N:7].O.C(=O)([O-])[O-:18].[Na+].[Na+]>C(O)C>[C:6]([C:8]1[CH:13]=[C:12]([CH2:14][OH:15])[CH:11]=[CH:10][N:9]=1)(=[O:18])[NH2:7]

参加物

6

反応物 4

HCID 962WaterHCID 6397ChlorotrimethylsilaneHCID 10340Sodium CarbonateHCID 107253914-(Hydroxymethyl)pyridine-2-carbonitrile2 回

生成物 1

HCID 230938024-(Hydroxymethyl)pyridine-2-carboxamide

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

反応条件

温度
50 °C

実験手順

Trimethylsilyl chloride (27 mL) and a suspension of 2-cyanopyridine-4-methanol (1.6 g, 11 mmol, Reference compound 11-1) in ethanol (20 mL) were added to ethanol (14mL) at room temperature under a nitrogen atmosphere, and then the mixture was stirred at 50° C. for 5.5 hours. The mixture was allowed to stand, and water (27 mL) and sodium carbonate (2.3 g, 22 mmol) were added thereto. The solvent was evaporated under reduced pressure, ethanol (100 mL) was added thereto, and the resulting insoluble matter was filtered out. The filtrate was evaporated under reduced pressure, then the resulting residue was dried at 50° C. under reduced pressure to the title reference compound including inorganic salt.

後処理

  1. customThe solvent was evaporated under reduced pressure, ethanol (100 mL)
  2. additionwas added
  3. filtrationthe resulting insoluble matter was filtered out
  4. customThe filtrate was evaporated under reduced pressure
  5. customthe resulting residue was dried at 50° C. under reduced pressure to the title reference compound

出典と根拠

ORDレコード
ord-cdcfdf070b644ea1a3303ae8e3bcdd4d
出典データセット
uspto-grants-2009_05
特許番号
US07534802B2

反応ノート

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