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

Hydrochloric Acid → HCID 86654325, 화합물

HRID 1404086
노트
인쇄 미리보기

반응식

HRID 1404086 반응식
[Br:1][C:2]1[CH:7]=[C:6]([F:8])[C:5]([N+:9]([O-])=O)=[C:4]([Br:12])[C:3]=1[O:13][CH3:14].Cl.Cl[Sn]Cl.O>C(O)C>[Br:12][C:4]1[C:3]([O:13][CH3:14])=[C:2]([Br:1])[CH:7]=[C:6]([F:8])[C:5]=1[NH2:9]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 225046691,3-Dibromo-5-fluoro-2-methoxy-4-nitrobenzeneHCID 43835034Tin dichloride dihydrate

생성물 1

HCID 86654325HCID 86654325, 화합물수율 100%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To the solution of 8-4 (234.2 g, 0.784 mol) and concentrated HCl (720 mL) in ethanol (2.2 L) at room temperature, SnCl2.H2O (415 g, 2.0 mol) was added by portions. The mixture was stirred for 16 h. TLC showed the reaction was completed. The volatiles were removed in vacuo. The residue was quenched with cooled water (500 mL) and ethyl acetate (1.5 L). The aqueous layer was neutralized with KOH until PH=6˜7. The white precipitate was filtered off to get a clear solution, which was extracted with ethyl acetate (600 mL×3). The combined organic layers were washed with brine twice, dried over anhydrous sodium sulfate. After filtration and evaporation, 8-5 (212.7 g, 100%) was obtained as brownish white solid.

후처리

  1. customThe volatiles were removed in vacuo
  2. customThe residue was quenched with cooled water (500 mL) and ethyl acetate (1.5 L)
  3. filtrationThe white precipitate was filtered off
  4. customto get a clear solution, which
  5. extractionwas extracted with ethyl acetate (600 mL×3)
  6. washThe combined organic layers were washed with brine twice
  7. dry with materialdried over anhydrous sodium sulfate
  8. filtrationAfter filtration and evaporation

출처 및 근거

ORD 기록
ord-a391756ec1f948629150018549acdcc5
출처 데이터셋
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08912220B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트