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

N-bromobutanimide → HCID 13649655, 화합물

HRID 280643
노트
인쇄 미리보기

반응식

HRID 280643 반응식
[Cl:1][C:2]1[CH:17]=[CH:16][C:5]([C:6]([C:8]2[CH:9]=[C:10]([CH3:15])[CH:11]=[CH:12][C:13]=2[Cl:14])=[O:7])=[CH:4][CH:3]=1.[Br:18]N1C(=O)CCC1=O>C1C=CC=CC=1.C(OOC(=O)C1C=CC=CC=1)(=O)C1C=CC=CC=1>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:6]([C:8]2[CH:9]=[C:10]([CH:11]=[CH:12][C:13]=2[Cl:14])[CH2:15][Br:18])=[O:7])=[CH:16][CH:17]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 67184N-bromobutanimideHCID 13649650HCID 13649650, 화합물

생성물 1

HCID 13649655HCID 13649655, 화합물수율 50.5%

시약·촉매·용매 2

HCID 7187Benzoyl Peroxide촉매HCID 241Benzene용매

실험 절차

A refluxing solution of 3-(4-chlorobenzoyl)-4-chlorotoluene (5.3 g, 20. mmol) and dibenzoylperoxide (200 mg, 0.83 mmol) in benzene (200 ml) was treated in portions with N-bromosuccinimide (4.4 g, 25. mmol) over 20 minutes. The mixture was refluxed 15 hours, cooled and filtered. The filtrate was evaporated under vacuum, triturated with diethyl ether (150 ml), filtered, and evaporated under vacuum. The residue was chromatographed on silica gel (500 g) eluted with 97:3 (v/v) n-hexane-ethyl acetate using a preparative high-performance liquid chromatograph to provide 3.47 g (50%) of 3-(4-chlorobenzoyl)-4-chlorobenzyl bromide, m.p. 81°-83° C.

후처리

  1. temperatureThe mixture was refluxed 15 hours
  2. temperaturecooled
  3. filtrationfiltered
  4. customThe filtrate was evaporated under vacuum
  5. customtriturated with diethyl ether (150 ml)
  6. filtrationfiltered
  7. customevaporated under vacuum
  8. customThe residue was chromatographed on silica gel (500 g)
  9. washeluted with 97:3 (v/v) n-hexane-ethyl acetate using a preparative high-performance liquid chromatograph

출처 및 근거

ORD 기록
ord-9f1e900c8a4a4ef4a9898a9c374a3f02
출처 데이터셋
uspto-grants-1986_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04590201

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트