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

Hydrochloric Acid → HCID 86646071, 화합물

HRID 1800674
노트
인쇄 미리보기

반응식

HRID 1800674 반응식
[C:1]([C:3]([C:6]1[CH:7]=[C:8]([C:12]([NH:14][C:15]2[CH:16]=[C:17]([NH:21][C:22]3[N:27]=[C:26]([S:28][C:29]#[N:30])[C:25]([N+:31]([O-])=O)=[CH:24][N:23]=3)[CH:18]=[CH:19][CH:20]=2)=[O:13])[CH:9]=[CH:10][CH:11]=1)([CH3:5])[CH3:4])#[N:2].CN1CCCC1=O.Cl.[OH-].[Na+]>C(O)C>[NH2:30][C:29]1[S:28][C:26]2[N:27]=[C:22]([NH:21][C:17]3[CH:16]=[C:15]([NH:14][C:12](=[O:13])[C:8]4[CH:9]=[CH:10][CH:11]=[C:6]([C:3]([C:1]#[N:2])([CH3:5])[CH3:4])[CH:7]=4)[CH:20]=[CH:19][CH:18]=3)[N:23]=[CH:24][C:25]=2[N:31]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 13387N-methyl-2-pyrrolidoneHCID 14798Sodium HydroxideHCID 86646070HCID 86646070, 화합물

생성물 1

HCID 86646071HCID 86646071, 화합물수율 60.4%

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
100 °C

실험 절차

To a suspension of 2-{[3-({[3-(1-cyano-1-methylethyl)phenyl]carbonyl}amino)phenyl]amino}-5-nitropyrimidin-4-yl thiocyanate (844 mg, 1.84 mmol) and reduced iron (513 mg, 9.20 mmol) in ethanol (16 mL)/1-methylpyrrolidin-2-one (8 mL) was added 1N hydrochloric acid (4 mL), and the mixture was stirred at 100° C. for 1.5 hr. The reaction mixture was neutralized with 2N aqueous sodium hydroxide solution (3 mL), and the insoluble material was filtered off. The filtrate was concentrated under reduced pressure. To the obtained residue was added saturated aqueous sodium hydrogen carbonate solution (50 mL), and the mixture was extracted with ethyl acetate (50 mL, 2×20 mL). The combined organic layer was washed with saturated brine (10 mL), and dried over anhydrous sodium sulfate. The insoluble material was filtered off, and the filtrate was concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (hexane/ethyl acetate=40/60→20/80), and the fractions containing the object product were concentrated under reduced pressure. The obtained residue was recrystallized from ethyl acetate and hexane to give the title compound (477 mg, 60%) as pale-purple crystals.

후처리

  1. filtrationthe insoluble material was filtered off
  2. concentrationThe filtrate was concentrated under reduced pressure
  3. additionTo the obtained residue was added saturated aqueous sodium hydrogen carbonate solution (50 mL)
  4. extractionthe mixture was extracted with ethyl acetate (50 mL, 2×20 mL)
  5. washThe combined organic layer was washed with saturated brine (10 mL)
  6. dry with materialdried over anhydrous sodium sulfate
  7. filtrationThe insoluble material was filtered off
  8. concentrationthe filtrate was concentrated under reduced pressure
  9. customThe obtained residue was purified by silica gel column chromatography (hexane/ethyl acetate=40/60→20/80)
  10. additionthe fractions containing the object product
  11. concentrationwere concentrated under reduced pressure
  12. customThe obtained residue was recrystallized from ethyl acetate and hexane

출처 및 근거

ORD 기록
ord-e817f42ba19b43b6aa1048b6172b8834
출처 데이터셋
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08344135B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트