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

Sodium hydride → 5-Bromo-2-(2-pyrrolidin-1-yl-ethoxy)-pyrimidine

HRID 888041
노트
인쇄 미리보기

반응식

HRID 888041 반응식
[OH:1][CH2:2][CH2:3][N:4]1[CH2:8][CH2:7][CH2:6][CH2:5]1.[Br:9][C:10]1[CH:11]=[N:12][C:13](Cl)=[N:14][CH:15]=1.[H-].[Na+]>CN(C=O)C>[Br:9][C:10]1[CH:11]=[N:12][C:13]([O:1][CH2:2][CH2:3][N:4]2[CH2:8][CH2:7][CH2:6][CH2:5]2)=[N:14][CH:15]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 762881-PyrrolidineethanolHCID 6066655-Bromo-2-chloropyrimidine

생성물 1

HCID 638675465-Bromo-2-(2-pyrrolidin-1-yl-ethoxy)-pyrimidine수율 38%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of N-2-hydroxyethylpyrrolidine (0.9 ml, 7.71 mmol) and 5-bromo-2-chloropyrimidine (1.2 g, 6.20 mmol), in DMF (7 ml), was added sodium hydride (60% in mineral oil, 0.35 g, 8.75 mmol). The mixture was stirred, under argon, at ambient temperature for 1 hour, before being heated to 90° C. and stirred for a further hour. The reaction mixture was then partitioned between ethyl acetate and water. The organics were separated, dried over magnesium sulfate and evaporated to dryness. The resultant oil was purified by flash chromatography on silica, eluting with an increasing gradient of methanol in dichloromethane (which contained 1% aqueous ammonia solution, 0.88 M) to give the title compound (640 mg, 38%); NMR Spectrum: (CDCl3) 1.76 (m, 4H), 2.39 (m, 4H), 3.90 (t, 2H), 4.48 (t, 2H), 8.50 (s, 2H); Mass Spectrum: M+H+ 272.

후처리

  1. temperaturebefore being heated to 90° C.
  2. stirringstirred for a further hour
  3. customThe reaction mixture was then partitioned between ethyl acetate and water
  4. customThe organics were separated
  5. dry with materialdried over magnesium sulfate
  6. customevaporated to dryness
  7. customThe resultant oil was purified by flash chromatography on silica
  8. washeluting with an increasing gradient of methanol in dichloromethane (which contained 1% aqueous ammonia solution, 0.88 M)

출처 및 근거

ORD 기록
ord-0844d7b57d664ae097e9cee74c7b12d9
출처 데이터셋
uspto-grants-2012_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08247562B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트