Potassium tert-butoxide → 2-Chloro-5H-pyrrolo[2,3-B]pyrazine

HRID 386407

反応式

HRID 386407 の反応式
CC(C)([O-])C.[K+].[Cl:7][C:8]1[N:9]=[C:10]([C:15]#[C:16][Si](CC)(CC)CC)[C:11]([NH2:14])=[N:12][CH:13]=1>CN1CCCC1=O.[Cl-].[Na+].O>[Cl:7][C:8]1[N:9]=[C:10]2[CH:15]=[CH:16][NH:14][C:11]2=[N:12][CH:13]=1

参加物

5

反応物 2

HCID 23665647Potassium tert-butoxideHCID 594635225-Chloro-3-(triethyl-silanylethynyl)-pyrazin-2-ylamine

生成物 1

HCID 457896382-Chloro-5H-pyrrolo[2,3-B]pyrazine

試薬・触媒・溶媒 2

HCID 13387N-methyl-2-pyrrolidone溶媒2 回HCID 57417360Sodium chloride; water溶媒

反応条件

温度
80 °C

実験手順

A solution of potassium tert-butoxide (1 g, 4.5 mM) in N-methylpyrrolidone (3 ml) was heated to 80° C. under nitrogen. A solution of 5-chloro-3-(triethyl-silanylethynyl)-pyrazin-2-ylamine (3) (1.2 g, 4.5 mmol) in N-methylpyrrolidone (10 ml) was added dropwise. The reaction mixture was stirred at 80° C. for a further fifty minutes and then the reaction mixture was allowed to cool to room temperature. Brine (10 ml) was added to the reaction mixture and extracted with ethyl acetate (5×20 ml). The combined organics were washed with brine, dried over magnesium sulfate and concentrated in vacuo to afford the title compound as a solution in N-methylpyrrolidone. MS (ES+): 154

後処理

  1. temperatureto cool to room temperature
  2. extractionextracted with ethyl acetate (5×20 ml)
  3. washThe combined organics were washed with brine
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-d8a8fc7882ee4968b2e53b2d95380ef9
出典データセット
uspto-grants-2013_02
特許番号
US08372835B2

関連ノート

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