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

Formamide → HCID 86639522, 화합물

HRID 1022410
노트
인쇄 미리보기

반응식

HRID 1022410 반응식
[CH:1]([NH2:3])=[O:2].[H-].[Na+].Cl[C:7]1[N:16]=[C:15]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[C:14]2[C:9](=[CH:10][CH:11]=[C:12]([Cl:23])[CH:13]=2)[N:8]=1.O>CN(C=O)C>[Cl:23][C:12]1[CH:13]=[C:14]2[C:9](=[CH:10][CH:11]=1)[N:8]=[C:7]([NH:3][CH:1]=[O:2])[N:16]=[C:15]2[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 713FormamideHCID 962WaterHCID 24758Sodium hydrideHCID 16282212,6-dichloro-4-phenylquinazoline

생성물 1

HCID 86639522HCID 86639522, 화합물수율 22.6%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of 54 mg of dry formamide in DMF (5 ml) was added 48 mg of sodium hydride (60%), followed by stirring at room temperature for 30 minutes. To the reaction mixture was added 275 mg of 2,6-dichloro-4-phenylquinazoline (compound No. II-2), followed by warming to 85° C. and further stirring for 3 hours. The resulting reaction solution was poured into 100 ml of water and extracted with ethyl acetate, and then extract was concentrated. The resulting residue was purified by silica gel column chromatography (ethyl acetate:hexane=1:3) to obtain 64 mg of the titled compound. Mp. 252.1° C. 1H NMR: 7.59-7.66 (3H, m), 7.72-7.81 (3H, m), 7.88 (1H, d, J=8.8 Hz), 8.02 (1H, d, J=2.0 Hz), 8.37 (1H, br. d, J=10.4 Hz), 9.71 (1H, d, J=10.4 Hz).

후처리

  1. temperatureby warming to 85° C.
  2. stirringfurther stirring for 3 hours
  3. customThe resulting reaction solution
  4. extractionextracted with ethyl acetate
  5. extractionextract
  6. concentrationwas concentrated
  7. customThe resulting residue was purified by silica gel column chromatography (ethyl acetate:hexane=1:3)

출처 및 근거

ORD 기록
ord-bf54ab31d7ad461eb6e7807937d9750c
출처 데이터셋
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08722580B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트