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

Methyl iodide → Ethyl 2-(5H-[1]benzopyrano[2,3-b]pyridin-7-yl)-2-cyanopropanoate

HRID 1579446
노트
인쇄 미리보기

반응식

HRID 1579446 반응식
[Na].[C:2]([CH2:4][C:5]1[CH:6]=[CH:7][C:8]2[O:17][C:12]3=[N:13][CH:14]=[CH:15][CH:16]=[C:11]3[CH2:10][C:9]=2[CH:18]=1)#[N:3].[C:19](=O)([O:23]CC)[O:20][CH2:21][CH3:22].[CH3:27]I>C(O)C>[C:2]([C:4]([C:5]1[CH:6]=[CH:7][C:8]2[O:17][C:12]3=[N:13][CH:14]=[CH:15][CH:16]=[C:11]3[CH2:10][C:9]=2[CH:18]=1)([CH3:27])[C:19]([O:20][CH2:21][CH3:22])=[O:23])#[N:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 6328Methyl iodideHCID 7766Diethyl CarbonateHCID 5360545SodiumHCID 12274195HCID 12274195, 화합물

생성물 1

HCID 21568495Ethyl 2-(5H-[1]benzopyrano[2,3-b]pyridin-7-yl)-2-cyanopropanoate

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A solution of 0.76 g of metallic sodium in 15 ml of ethanol is added to a mixture of 6.6 g of 7-cyanomethyl-5H-[1]benzopyrano[2,3-b]pyridine and 46 ml of diethyl carbonate, and the whole mixture is refluxed for 1 hour. After cooling, 5.2 g of methyl iodide is added to the reaction mixture. The temperature of the mixture is raised gradually, and the mixture is refluxed for 2 hours. The excess diethyl carbonate is distilled off, and toluene is added to the residue. The mixture is washed with water, and the toluene layer is dried. The toluene is distilled off, and the residue is recrystallized from isopropyl alcohol to give ethyl 2-cyano-2-(5H-[1]benzopyrano-[2,3-b]pyridin-7-yl)propionate melting at 119°-120°C.

후처리

  1. temperaturethe whole mixture is refluxed for 1 hour
  2. temperatureAfter cooling
  3. temperatureThe temperature of the mixture is raised gradually
  4. temperaturethe mixture is refluxed for 2 hours
  5. distillationThe excess diethyl carbonate is distilled off
  6. additiontoluene is added to the residue
  7. washThe mixture is washed with water
  8. dry with materialthe toluene layer is dried
  9. distillationThe toluene is distilled off
  10. customthe residue is recrystallized from isopropyl alcohol

출처 및 근거

ORD 기록
ord-aaf08c8efa8c415a8d5640f0bbe123f7
출처 데이터셋
uspto-grants-1976_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03931205

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트