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

1,3-Dibromobenzene → 4-(3-bromophenyl)-N,N-dimethylmorpholine-2-carboxamide

HRID 1914044
노트
인쇄 미리보기

반응식

HRID 1914044 반응식
Br[C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Br:8])[CH:3]=1.[CH3:9][N:10]([CH3:19])[C:11]([CH:13]1[O:18][CH2:17][CH2:16][NH:15][CH2:14]1)=[O:12].C1C=CC(P(C2C(C3C(P(C4C=CC=CC=4)C4C=CC=CC=4)=CC=C4C=3C=CC=C4)=C3C(C=CC=C3)=CC=2)C2C=CC=CC=2)=CC=1.CC([O-])(C)C.[Na+]>C1(C)C=CC=CC=1.C(Cl)Cl.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd]>[Br:8][C:4]1[CH:3]=[C:2]([N:15]2[CH2:16][CH2:17][O:18][CH:13]([C:11]([N:10]([CH3:19])[CH3:9])=[O:12])[CH2:14]2)[CH:7]=[CH:6][CH:5]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 79271,3-DibromobenzeneHCID 634876Binap, (A+-)-HCID 20472122N,N-dimethylmorpholine-2-carboxamideHCID 23676156Sodium t-butoxide

생성물 1

HCID 711388204-(3-bromophenyl)-N,N-dimethylmorpholine-2-carboxamide수율 42.3%

시약·촉매·용매 3

HCID 9811564
Bis(dibenzylideneacetone)palladium
촉매
HCID 1140Toluene용매
HCID 6344Dichloromethane용매

반응 조건

온도
80 °C

실험 절차

A mixture of 1,3-dibromobenzene (387 μL, 3.20 mmol), N,N-dimethylmorpholine-2-carboxamide (506 mg, 3.20 mmol), Pd2(dba)3 (73.3 mg, 0.0800 mmol), rac-BINAP (154 mg, 0.240 mmol) and NaOtBu (369 mg, 3.84 mmol) in toluene (8 mL) was heated at 80° C. for 5 hours under nitrogen. After cooling to room temperature, the mixture was diluted with DCM and filtered through a Celite pad. The combined filtrate and washings were concentrated. The residue was purified by silica gel column chromatography (EtOAc/hexane=95:5→90:10→80:20→67:33→50:50) to afford desired product (424 mg, 42.3%) as orange oil.

후처리

  1. temperatureAfter cooling to room temperature
  2. filtrationfiltered through a Celite pad
  3. concentrationThe combined filtrate and washings were concentrated
  4. customThe residue was purified by silica gel column chromatography (EtOAc/hexane=95:5→90:10→80:20→67:33→50:50)

출처 및 근거

ORD 기록
ord-55db98e3a3f64b9e8948c98a933c06fa
출처 데이터셋
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08609688B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트