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

Triphenyl phosphite → 1-(1-Bromo-2,2,2-trifluoroethyl)-3,5-dichlorobenzene

HRID 1502655
노트
인쇄 미리보기

반응식

HRID 1502655 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([CH:9](O)[C:10]([F:13])([F:12])[F:11])[CH:5]=[C:6]([Cl:8])[CH:7]=1.[Br:15]N1C(=O)CCC1=O.P(OC1C=CC=CC=1)(OC1C=CC=CC=1)OC1C=CC=CC=1>C(Cl)Cl>[Br:15][CH:9]([C:4]1[CH:3]=[C:2]([Cl:1])[CH:7]=[C:6]([Cl:8])[CH:5]=1)[C:10]([F:13])([F:12])[F:11]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 7540Triphenyl phosphiteHCID 67184N-bromobutanimideHCID 616446851-(3,5-Dichlorophenyl)-2,2,2-trifluoroethanol

생성물 1

HCID 866751181-(1-Bromo-2,2,2-trifluoroethyl)-3,5-dichlorobenzene수율 40%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
25 °C

실험 절차

To a stirred solution of 1-(3,5-dichlorophenyl)-2,2,2-trifluoroethanol (4.0 g, 16.3 mmol) in CH2Cl2 (50 mL), were added N-bromosuccinimide (NBS; 2.9 g, 16.3 mmol) and triphenyl phosphite (5.06 g, 16.3 mmol), and the resultant reaction mixture was heated at reflux for 18 h. After the reaction was deemed complete by TLC, the reaction mixture was cooled to 25° C. and was concentrated under reduced pressure. Purification by flash column chromatography (SiO2, 100-200 mesh; eluting with 100% pentane) afforded the title compound as a liquid (2.0 g, 40%): 1H NMR (400 MHz, CDCl3) δ 7.41 (s, 3H), 5.00 (m, 1H); EIMS m/z 306 ([M]+).

후처리

  1. customthe resultant reaction mixture
  2. temperaturewas heated
  3. temperatureat reflux for 18 h
  4. concentrationwas concentrated under reduced pressure
  5. customPurification
  6. washby flash column chromatography (SiO2, 100-200 mesh; eluting with 100% pentane)

출처 및 근거

ORD 기록
ord-f693ee922c9d4a3cac112306c1913564
출처 데이터셋
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09210927B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트