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

HRID 43248

반응식

HRID 43248 반응식
[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

참가 물질

4

반응물 2

HCID 8022Ethyl isocyanate2회HCID 866355376-Chloro-pyrido[2,3-b]pyrazin-3-ylamine

생성물 1

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

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

반응 조건

온도
100 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-5d1edd0bd74442209dc5845b91c37678
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08536332B2

연결된 노트

불러오는 중…