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

Dimethylformamide → 2-[1-(4-amino-3-nitrophenyl)ethenyl]-N-[3-(trifluoromethyl)phenyl]benzamide

HRID 2367118
노트
인쇄 미리보기

반응식

HRID 2367118 반응식
Cl[C:2]1[CH:7]=[CH:6][C:5]([C:8]([C:10]2[CH:28]=[CH:27][CH:26]=[CH:25][C:11]=2[C:12]([NH:14][C:15]2[CH:20]=[CH:19][CH:18]=[C:17]([C:21]([F:24])([F:23])[F:22])[CH:16]=2)=[O:13])=[CH2:9])=[CH:4][C:3]=1[N+:29]([O-:31])=[O:30].[N-:32]=[N+]=[N-].[Na+].CN(C)C=O.[BH4-].[Na+]>C(OCC)(=O)C.O1CCCC1>[NH2:32][C:2]1[CH:7]=[CH:6][C:5]([C:8]([C:10]2[CH:28]=[CH:27][CH:26]=[CH:25][C:11]=2[C:12]([NH:14][C:15]2[CH:20]=[CH:19][CH:18]=[C:17]([C:21]([F:24])([F:23])[F:22])[CH:16]=2)=[O:13])=[CH2:9])=[CH:4][C:3]=1[N+:29]([O-:31])=[O:30]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 6228DimethylformamideHCID 33557Sodium AzideHCID 4311764Sodium borohydrideHCID 67045429HCID 67045429, 화합물

생성물 1

HCID 670444852-[1-(4-amino-3-nitrophenyl)ethenyl]-N-[3-(trifluoromethyl)phenyl]benzamide수율 50%

시약·촉매·용매 2

HCID 8028
Tetrahydrofuran
용매
HCID 8857Ethyl Acetate용매

반응 조건

온도
60 °C

실험 절차

A mixture of 2-[1-(4-chloro-3-nitrophenyl)ethenyl]-N-[3-(trifluoromethyl)phenyl]benzamide (0.72 g, 1.6 mmol), sodium azide (3.1 g, 4.8 mmol) and N,N-dimethylformamide (2 mL) was stirred 60° C. for 18 hours. The reaction mixture was diluted with ethyl acetate (50 mL), washed with water (3×30 mL), brine (30 mL), dried over sodium sulfate, filtered and concentrated to give an oily residue. This residue was dissolved in tetrahydrofuran, cooled to 0° C. then sodium borohydride (0.11 g, 2.7 mmol) was added and stirring was continued for 30 minutes at room temperature. The reaction mixture was quenched with methanol (2 mL), concentrated then diluted with ethyl acetate (50 mL). The organic solution was washed with water (30 mL) then brine solution (30 mL) then dried over sodium sulfate, filtered and concentrated. The residue was purified by flash chromatography (silica gel, eluting with 15-50% ethyl acetate-hexane) to give 2-[1-(4-amino-3-nitrophenyl)ethenyl]-N-[3-(trifluoromethyl)phenyl]benzamide (0.35 g, 0.8 mmol, 50% yield). MS (EI) for C22H16F3N3O3: 428 (MH+).

후처리

  1. washwashed with water (3×30 mL), brine (30 mL)
  2. dry with materialdried over sodium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customto give an oily residue
  6. temperaturecooled to 0° C.
  7. stirringstirring
  8. waitwas continued for 30 minutes at room temperature
  9. customThe reaction mixture was quenched with methanol (2 mL)
  10. concentrationconcentrated
  11. additionthen diluted with ethyl acetate (50 mL)
  12. washThe organic solution was washed with water (30 mL)
  13. dry with materialbrine solution (30 mL) then dried over sodium sulfate
  14. filtrationfiltered
  15. concentrationconcentrated
  16. customThe residue was purified by flash chromatography (silica gel, eluting with 15-50% ethyl acetate-hexane)

출처 및 근거

ORD 기록
ord-283cfd33120045df85d726cfe31b4811
출처 데이터셋
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08697737B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트