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

Isopropanol → 6-Oxo-1,6-dihydro-3,4'-bipyridine-5-carbonitrile

HRID 27765
노트
인쇄 미리보기

반응식

HRID 27765 반응식
[CH:1]([OH:4])([CH3:3])C.C[N:6](C)[CH:7]=[C:8]([C:11]1[CH:16]=[CH:15][N:14]=[CH:13][CH:12]=1)[CH:9]=O.C(#N)C[C:20]#[N:21]>O>[C:20]([C:3]1[C:1](=[O:4])[NH:6][CH:7]=[C:8]([C:11]2[CH:16]=[CH:15][N:14]=[CH:13][CH:12]=2)[CH:9]=1)#[N:21]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 3776Isopropanol2회HCID 8010MalononitrileHCID 541977173-Dimethylamino-2-(4-pyridinyl)acrolein

생성물 1

HCID 1319896-Oxo-1,6-dihydro-3,4'-bipyridine-5-carbonitrile

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
3 °C

실험 절차

To 2500 ml of isopropyl alcohol heated to reflux was added with stirring 300 g of 3-dimethylamino-2-(4-pyridinyl)-2-propen-1-one [same as α-(4-pyridinyl)-β-(dimethyl-amino)acrolein]. To the resulting mixture was added 500 ml of a solution containing 138 g of malonontrile, 1500 ml of isopropyl alcohol and 100 ml of water. The temperature was brought back to reflux in about 10 minutes and then the remainder of the malononitrile solution was added from a dropping funnel over a period of about 25 minutes. The reaction mixture was stirred at reflux for additional 35 minutes and the resulting orange suspension was cooled to 3° C. The precipitated solid was collected by filtration and the filter cake was washed with four 100 ml portions of cold isopropyl alcohol. The solid was then dried at 40° C. in vacuo overnight (about 15 hours) and then for two hours at 60° C. to yield 245 g of 5-cyano[3,4'-bipyridin]-6(1H)-one [same as 1,2-dihydro-2-oxo-5-(4-pyridinyl)nicotinonitrile], m.p.>300° C. The nuclear magnetic resonance spectrum of this product was consistent with that of the same product prepared by another method. The filtrate was concentrated in vacuo to about 500 ml volume and cooled in an ice bath. A total of 40 g of a second crop material was obtained, m.p.>300° C.

후처리

  1. temperatureto reflux
  2. additionwas added
  3. temperatureto reflux in about 10 minutes
  4. temperatureat reflux for additional 35 minutes
  5. filtrationThe precipitated solid was collected by filtration
  6. washthe filter cake was washed with four 100 ml portions of cold isopropyl alcohol
  7. customThe solid was then dried at 40° C. in vacuo overnight (about 15 hours)

출처 및 근거

ORD 기록
ord-fccf062ecd7243b283bbcc9cce2c66ce
출처 데이터셋
uspto-grants-1980_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04223149

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트