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

Triethylamine → 1-(3-Fluorobenzoyl)pyrazolidin-3-one

HRID 1629972
노트
인쇄 미리보기

반응식

HRID 1629972 반응식
[NH:1]1[CH2:5][CH2:4][C:3](=[O:6])[NH:2]1.[F:7][C:8]1[CH:9]=[C:10]([CH:14]=[CH:15][CH:16]=1)[C:11](O)=[O:12].C(N(CC)CC)C.CCCP1(OP(CCC)(=O)OP(CCC)(=O)O1)=O>ClCCl>[F:7][C:8]1[CH:9]=[C:10]([CH:14]=[CH:15][CH:16]=1)[C:11]([N:1]1[CH2:5][CH2:4][C:3](=[O:6])[NH:2]1)=[O:12]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 99683-Fluorobenzoic AcidHCID 111923Propylphosphonic anhydrideHCID 1514973-Pyrazolidone

생성물 1

HCID 711848671-(3-Fluorobenzoyl)pyrazolidin-3-one수율 32,422.5%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of pyrazolidin-3-one (6.9 gm, 0.080 mmol, 1 equiv.) in dry dichloromethane (70 ml), 3-fluorobenzoic acid (12.3 gm, 0.088 mmol, 1.1 equiv.), triethylamine (24.3 gm, 0.240 mmol, 3 equiv.) and 1-propane phosphonic acid cyclic anhydride (60% by weight in ethyl acetate) (51 gm, 0.16 mmol, 2 equiv.) were added in cooling condition and stirred for overnight at room temperature. The reaction mixture was concentrated and the residue was poured in water (500 ml), extracted with dichloromethane (100 ml×2) and concentrated. The crude product was purified by silica gel column using (60-120) mesh to get the pure product as yellow oil (5.4 gm, 32% yield).

후처리

  1. temperaturein cooling condition
  2. concentrationThe reaction mixture was concentrated
  3. additionthe residue was poured in water (500 ml)
  4. extractionextracted with dichloromethane (100 ml×2)
  5. concentrationconcentrated
  6. customThe crude product was purified by silica gel column

출처 및 근거

ORD 기록
ord-3e10c8ac1cd74efbaed5448a27f5b0dc
출처 데이터셋
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08791114B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트