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

Water → Ethyl 2-[2-(2,4-difluorophenylamino)-5-fluoro-6-(1-piperazinyl)nicotinoyl]acetate

HRID 232468
노트
인쇄 미리보기

반응식

HRID 232468 반응식
[NH:1]1[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.[F:7][C:8]1[CH:13]=[C:12]([F:14])[CH:11]=[CH:10][C:9]=1[NH:15][C:16]1[N:29]=[C:28](OS(C2C(C)=CC(C)=CC=2C)(=O)=O)[C:27]([F:43])=[CH:26][C:17]=1[C:18]([CH2:20][C:21]([O:23][CH2:24][CH3:25])=[O:22])=[O:19].C(OCC)(=O)C.O>C(Cl)Cl.CCCCCC>[F:7][C:8]1[CH:13]=[C:12]([F:14])[CH:11]=[CH:10][C:9]=1[NH:15][C:16]1[N:29]=[C:28]([N:1]2[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]2)[C:27]([F:43])=[CH:26][C:17]=1[C:18]([CH2:20][C:21]([O:23][CH2:24][CH3:25])=[O:22])=[O:19]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 962WaterHCID 4837PiperazineHCID 8857Ethyl AcetateHCID 13849317Ethyl 2-[2-(2,4-difluorophenylamino)-5-fluoro-6-(2,4,6-trimethylbenzenesulfonyloxy)nicotinoyl]acetate

생성물 1

HCID 13922529Ethyl 2-[2-(2,4-difluorophenylamino)-5-fluoro-6-(1-piperazinyl)nicotinoyl]acetate수율 69.9%

시약·촉매·용매 2

HCID 6344
Dichloromethane
용매
HCID 8058Hexane용매

실험 절차

In 2 ml of methylene chloride was dissolved 130 mg of anhydrous piperazine, and 200 mg of ethyl 2-[2-(2,4-difluorophenylamino)-5-fluoro-6-(2,4,6-trimethylbenzenesulfonyloxy)nicotinoyl]acetate was added thereto with ice-cooling, after which the resulting mixture was subjected to reaction at the same temperature for 40 minutes. Subsequently, the reaction mixture was added to a mixture of 10 ml of ethyl acetate and 10 ml of water, and the organic layer was separated, washed successively with 2 ml of saturated aqueous sodium hydrogencarbonate solution and 2 ml of saturated aqueous sodium chloride solution, and then dried over anhydrous magnesium sulfate. The solvent was removed by distillation under reduced pressure, and to the crystalline material thus obtained was added 1 ml of n-hexane, after which crystals were collected by filtration to obtain 110 mg (yield 69.9%) of ethyl 2-[2-(2,4-difluorophenylamino)-5-fluoro-6-(1-piperazinyl)nicotinoyl]acetate. The physical properties of this compound were identical with those of the compound obtained in Example 30.

후처리

  1. additionwas added
  2. temperaturewith ice-cooling
  3. customafter which the resulting mixture was subjected to reaction at the same temperature for 40 minutes
  4. customthe organic layer was separated
  5. washwashed successively with 2 ml of saturated aqueous sodium hydrogencarbonate solution and 2 ml of saturated aqueous sodium chloride solution
  6. dry with materialdried over anhydrous magnesium sulfate
  7. customThe solvent was removed by distillation under reduced pressure
  8. customto the crystalline material thus obtained
  9. filtrationafter which crystals were collected by filtration

출처 및 근거

ORD 기록
ord-6f9ca15588384edab4dcb97d98ae9697
출처 데이터셋
uspto-grants-1989_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04851535

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트