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

2,2'-Bipyridine → 6-Phenyl-2,2'-bipyridine

HRID 2117813
노트
인쇄 미리보기

반응식

HRID 2117813 반응식
[C:1]1([Li])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C1CCCCC1.C(OCC)C.[N:19]1[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=1[C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][N:26]=1.C(OCC)C>O>[C:1]1([C:27]2[N:26]=[C:25]([C:20]3[CH:21]=[CH:22][CH:23]=[CH:24][N:19]=3)[CH:30]=[CH:29][CH:28]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 14742,2'-BipyridineHCID 3283Diethyl EtherHCID 21895417Cyclohexane diethyletherHCID 178506676HCID 178506676, 화합물

생성물 1

HCID 46132696-Phenyl-2,2'-bipyridine수율 55.4%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A solution of phenyllithium.cyclohexane/diethyl ether (40.9 ml, 38.4 mmol) was dropwise added to a mixture of 2,2′-bipyridine (5.0 g, 32.0 mmol) and diethyl ether (50 ml) at 5° C. while 15 minutes. This reaction mixture was stirred at room temperature for 2 hours, then the mixture was poured into water, an organic layer was separated from the mixture, furthermore an aqueous layer was extracted with dichloromethane. The organic layer was combined, and the solvent was distilled off, and the residue was diluted with acetone (50 ml), then saturated potassium permanganate acetone solution (120 ml) was added thereto, the mixture was stirred at room temperature for 1 hour. The obtained reaction mixture was filtered by Celite, the solvent of the filtrate was distilled off, and the residue was purified by silica gel column chromatography and recrystallization, thereby obtaining 4.2 g of 6-phenyl-2,2′-bipyridine as white crystal. Yield: 55.4%.

후처리

  1. customan organic layer was separated from the mixture
  2. extractionfurthermore an aqueous layer was extracted with dichloromethane
  3. distillationthe solvent was distilled off
  4. additionthe residue was diluted with acetone (50 ml)
  5. additionsaturated potassium permanganate acetone solution (120 ml) was added
  6. stirringthe mixture was stirred at room temperature for 1 hour
  7. customThe obtained reaction mixture
  8. filtrationwas filtered by Celite
  9. distillationthe solvent of the filtrate was distilled off
  10. customthe residue was purified by silica gel column chromatography and recrystallization

출처 및 근거

ORD 기록
ord-7964872ef94b4462aa6cb83eb4999bbc
출처 데이터셋
uspto-grants-2008_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07442797B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트