홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Ethanol → HCID 178507684, 화합물

HRID 26405
노트
인쇄 미리보기

반응식

HRID 26405 반응식
[NH2:1][C:2]1[N:7]=[C:6]([NH2:8])[CH:5]=[C:4]([Cl:9])[N:3]=1.C([OH:12])C.C(OO)(=O)C>C(O)(=O)C>[NH2:1][C:2]1[N+:7]([O-:12])=[C:6]([NH2:8])[CH:5]=[C:4]([Cl:9])[N:3]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 702EthanolHCID 6585Peracetic AcidHCID 674322,4-Diamino-6-chloropyrimidine

생성물 1

HCID 178507684HCID 178507684, 화합물

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
35 °C

실험 절차

144.5 G. of 2,4-diamino-6-chloropyrimidine are suspended in 2000 ml. of ethanol. The suspension is warmed to 35° C. while stirring (about 15 minutes), the greater part of the material passing into solution. This mixture is then cooled down to 6°-8° C. and at this temperature there are added dropwise within 40 minutes 175 ml. of 40% peracetic acid in glacial acetic acid. After completion of the addition, the mixture is stirred at 6°-8° C. for a further 30 minutes. Thereafter, the mixture is left to warm up to room temperature, and stirred at this temperature for 3 hours. 2000 Ml. of petroleum ether are added, the mixture is stirred for 1 hour and then left to stand overnight. The separated precipitate is filtered off, back-washed with 200 ml. of petroleum ether and dried under reduced pressure, there being obtained 2,4-diamino-6-chloro-pyrimidine-3-oxide. Recrystallization yields analytically pure product having a melting point of 193° C.

후처리

  1. temperatureThis mixture is then cooled down to 6°-8° C. and at this temperature there
  2. additionare added dropwise within 40 minutes 175 ml
  3. additionAfter completion of the addition
  4. stirringthe mixture is stirred at 6°-8° C. for a further 30 minutes
  5. waitThereafter, the mixture is left
  6. temperatureto warm up to room temperature
  7. stirringstirred at this temperature for 3 hours
  8. stirringthe mixture is stirred for 1 hour
  9. waitleft
  10. waitto stand overnight
  11. filtrationThe separated precipitate is filtered off
  12. washback-washed with 200 ml
  13. dry with materialof petroleum ether and dried under reduced pressure, there

출처 및 근거

ORD 기록
ord-8e32e366e0bb464a9c23ca4d3634022b
출처 데이터셋
uspto-grants-1979_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04150131

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트