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

Dimethylformamide → 3-((4-Iodo-1H-pyrazol-1-yl)methyl)-5-methylisoxazole

HRID 2205869
노트
인쇄 미리보기

반응식

HRID 2205869 반응식
[I:1][C:2]1[CH:3]=[N:4][NH:5][CH:6]=1.Br[CH2:8][C:9]1[CH:13]=[C:12]([CH3:14])[O:11][N:10]=1.C(=O)([O-])[O-].[K+].[K+].CN(C=O)C>C(OCC)(=O)C>[I:1][C:2]1[CH:3]=[N:4][N:5]([CH2:8][C:9]2[CH:13]=[C:12]([CH3:14])[O:11][N:10]=2)[CH:6]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 11430Potassium CarbonateHCID 770224-IodopyrazoleHCID 27763043-(Bromomethyl)-5-methylisoxazole

생성물 1

HCID 644297653-((4-Iodo-1H-pyrazol-1-yl)methyl)-5-methylisoxazole수율 56.8%

시약·촉매·용매 1

HCID 8857Ethyl Acetate
용매

실험 절차

4-Iodo-1H-pyrazole (0.826 g, 4.26 mmol) (1), 3-(bromomethyl)-5-methylisoxazole (0.75 g, 4.26 mmol) and potassium carbonate (1.18 g, 8.52 mmol) were added to dry DMF (8 ml) and stirred at room temperature for 16 h. The reaction was diluted with ethyl acetate (20 ml) and washed with water, brine and dried. The organic solution was concentrated in vacuo and the residue purified by flash silica chromatography (20% ethyl acetate in hexane). The pure fractions provided the title compound as a white powder (0.7 g, 56.8%). 1H-NMR (500 MHz, CDCl3) 2.4 (s, 3H), 5.33 (s, 2H), 5.92 (s, 1H), 7.51 (s, 1H), 7.55 (s, 1H).

후처리

  1. washwashed with water, brine
  2. customdried
  3. concentrationThe organic solution was concentrated in vacuo
  4. customthe residue purified by flash silica chromatography (20% ethyl acetate in hexane)

출처 및 근거

ORD 기록
ord-dddfd510e75f4bc4b236c5ead7a13f93
출처 데이터셋
uspto-grants-2016_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09371319B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트