Ethyl isocyanate → 1-(6-Chloro-pyrido[2,3-b]pyrazin-3-yl)-3-ethyl-urea

HRID 220132

反応式

HRID 220132 の反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[C:6]([N:12]=1)=[N:7][C:8]([NH2:11])=[CH:9][N:10]=2.[CH2:13]([N:15]=[C:16]=[O:17])[CH3:14]>O1CCOCC1>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[C:6]([N:12]=1)=[N:7][C:8]([NH:11][C:16]([NH:15][CH2:13][CH3:14])=[O:17])=[CH:9][N:10]=2

参加物

4

反応物 2

HCID 8022Ethyl isocyanate2 回HCID 866355376-Chloro-pyrido[2,3-b]pyrazin-3-ylamine

生成物 1

HCID 579472491-(6-Chloro-pyrido[2,3-b]pyrazin-3-yl)-3-ethyl-urea収率 93.3%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

反応条件

温度
100 °C

実験手順

A total of 5.0 g 6-Chloro-pyrido[2,3-b]pyrazin-3-ylamine (27.7 mmol; 1 eq) was suspended in 150 mL of dry 1,4-dioxane. 2.63 g (33.2 mmol; 1.2 eq) ethyl isocyanate was added and the reaction mixture was stirred at 100° C. for 4 hours. Additional 1.97 g (27.7 mmol; 1 eq) of ethyl isocyanate were added and the resulting solution was stirred at 100° C. for further 4 hours. After cooling to room temperature, the precipitate was filtered of and dried in vacuo to afford 6.5 g (93.3% yield) of 1-(6-Chloro-pyrido[2,3-b]pyrazin-3-yl)-3-ethyl-urea.

後処理

  1. stirringthe resulting solution was stirred at 100° C. for further 4 hours
  2. temperatureAfter cooling to room temperature
  3. filtrationthe precipitate was filtered of and
  4. customdried in vacuo

出典と根拠

ORDレコード
ord-85f785c86c5a49b48dd855b73c947801
出典データセット
uspto-grants-2012_06
特許番号
US08202883B2

関連ノート

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