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

Sulfuric Acid → [7-[3-(Ethylamino)phenyl]pyrazolo[1,5-a]pyrimidin-3-yl]-2-furanylmethanone

HRID 1247968
노트
인쇄 미리보기

반응식

HRID 1247968 반응식
[CH2:1]([N:3]([C:14]1[CH:19]=[CH:18][CH:17]=[C:16]([C:20]2[N:25]3[N:26]=[CH:27][C:28]([C:29]([C:31]4[O:32][CH:33]=[CH:34][CH:35]=4)=[O:30])=[C:24]3[N:23]=[CH:22][CH:21]=2)[CH:15]=1)S(C1C=CC(C)=CC=1)(=O)=O)[CH3:2].S(=O)(=O)(O)O.[OH-].[NH4+]>O>[CH2:1]([NH:3][C:14]1[CH:15]=[C:16]([C:20]2[N:25]3[N:26]=[CH:27][C:28]([C:29]([C:31]4[O:32][CH:33]=[CH:34][CH:35]=4)=[O:30])=[C:24]3[N:23]=[CH:22][CH:21]=2)[CH:17]=[CH:18][CH:19]=1)[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 1118Sulfuric AcidHCID 14923Ammonium HydroxideHCID 20280467N-ethyl-N-[3-[3-(2-furanylcarbonyl)pyrazolo[1,5-a]pyrimidin-7-yl]phenyl]-4-methylbenzenesulfonamide

생성물 1

HCID 13475999[7-[3-(Ethylamino)phenyl]pyrazolo[1,5-a]pyrimidin-3-yl]-2-furanylmethanone

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A 10.7 g portion of N-ethyl-N-[3-[3-(2-furanylcarbonyl)pyrazolo[1,5-a]pyrimidin-7-yl]phenyl]-4-methylbenzenesulfonamide was added to a mixture of 90 ml of water and 210 ml of concentrated sulfuric acid. This mixture was heated to 140°-145° C., allowed to cool slowly to room temperature, then cooled to -10° C., poured onto ice, made basic with 550 ml of concentrated ammonium hydroxide and cooled to 0° C. This mixture was extracted with dichloromethane. The extract was passed through hydrous magnesium silicate and washed with 200 ml of dichloromethane. The dichloromethane filtrate and wash was combined with 300 ml of hexane, concentrated to 300 ml, diluted to 800 ml with hexane, treated with charcoal, clarified and cooled to -10° C. This material was filtered, the filtrate concentrated to turbidity and cooled at -10° C. The precipitate was collected, washed with hexane and dried at 60° C. in vacuo, giving 2.3 g of the desired product, mp 142°-143° C.

후처리

  1. temperatureThis mixture was heated to 140°-145° C.
  2. temperaturecooled to -10° C.
  3. additionpoured onto ice
  4. temperaturecooled to 0° C
  5. extractionThis mixture was extracted with dichloromethane
  6. washwashed with 200 ml of dichloromethane
  7. washThe dichloromethane filtrate and wash
  8. concentrationconcentrated to 300 ml
  9. additiondiluted to 800 ml with hexane
  10. additiontreated with charcoal
  11. temperaturecooled to -10° C
  12. filtrationThis material was filtered
  13. concentrationthe filtrate concentrated to turbidity
  14. temperaturecooled at -10° C
  15. customThe precipitate was collected
  16. washwashed with hexane
  17. customdried at 60° C. in vacuo

출처 및 근거

ORD 기록
ord-6e58576fa90d407d940edf49071d3708
출처 데이터셋
uspto-grants-1985_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04521422

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트