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

Chloroform → 3-Bromo-2,5-bis(4-methoxyphenyl)thiophene

HRID 708308
노트
인쇄 미리보기

반응식

HRID 708308 반응식
Br[C:2]1[S:3][C:4](Br)=[CH:5][C:6]=1[Br:7].[CH3:9][O:10][C:11]1[CH:16]=[CH:15][C:14](B(O)O)=[CH:13][CH:12]=1.[C:20](=[O:23])([O-])[O-].[Na+].[Na+].C(Cl)(Cl)Cl>C1COCC1.O.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.CCOC(C)=O>[Br:7][C:6]1[CH:5]=[C:4]([C:14]2[CH:15]=[CH:16][C:11]([O:10][CH3:9])=[CH:12][CH:13]=2)[S:3][C:2]=1[C:11]1[CH:16]=[CH:15][C:14]([O:23][CH3:20])=[CH:13][CH:12]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 6212ChloroformHCID 10340Sodium CarbonateHCID 76592Thiophene, 2,3,5-tribromo-HCID 201262(4-Methoxyphenyl)boronic acid

생성물 1

HCID 679735003-Bromo-2,5-bis(4-methoxyphenyl)thiophene수율 65%

시약·촉매·용매 3

HCID 178418397
HCID 178418397, 화합물
촉매
HCID 8857Ethyl Acetate용매
HCID 21881883Oxolane--water (1/1)용매

실험 절차

2,3,5-Tribromothiophene (6.42 g, 20 mmol), 4-methoxyphenylboronic acid (6.38 g, 42 mmol) and sodium carbonate (8.5 g, 80 mmol) were stirred in THF/water mixture (125/50 ml) for 90 min at RT under argon flushing. Pd(PPh3)4 (693 mg, 0.6 mmol) was added. The mixture was refluxed for 16 h (TLC), cooled to RT and THF was removed by evaporation. Water was added and aqueous fractions extracted with EtOAc. The organic fractions were combined, solvent removed and the crude product purified by flash chromatography (Silica gel; hexane/chloroform/EtOAc; gradient up to 20% chloroform then 20% EtOAc) to yield 3-bromo-2,5-bis(4-methoxyphenyl)thiophene (4.9 g, 13 mmol, 65%).

후처리

  1. temperatureThe mixture was refluxed for 16 h (TLC)
  2. customTHF was removed by evaporation
  3. additionWater was added
  4. extractionaqueous fractions extracted with EtOAc
  5. customsolvent removed
  6. customthe crude product purified by flash chromatography (Silica gel

출처 및 근거

ORD 기록
ord-4ad2ec4d58e54e07bd01dbcc2fa5da29
출처 데이터셋
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09176357B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트