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

o-Iodonitrobenzene → 6-(2-Nitrophenyl)-2,3-dimethoxy-7,8-dihydronaphthalene

HRID 1582869
노트
인쇄 미리보기

반응식

HRID 1582869 반응식
C([O-])(=O)C.[Na+].[CH3:6][O:7][C:8]1[CH:9]=[C:10]2[C:15](=[CH:16][C:17]=1[O:18][CH3:19])[CH:14]=[CH:13][CH2:12][CH2:11]2.I[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=1[N+:27]([O-:29])=[O:28]>CC(N(C)C)=O.Cl[Pd](Cl)([P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1>[N+:27]([C:22]1[CH:23]=[CH:24][CH:25]=[CH:26][C:21]=1[C:12]1[CH2:13][CH2:14][C:15]2[CH:16]=[C:17]([O:18][CH3:19])[C:8]([O:7][CH3:6])=[CH:9][C:10]=2[CH:11]=1)([O-:29])=[O:28]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 69115o-IodonitrobenzeneHCID 517045Sodium AcetateHCID 127653926,7-Dimethoxy-3,4-dihydronaphthalene

생성물 1

HCID 227164386-(2-Nitrophenyl)-2,3-dimethoxy-7,8-dihydronaphthalene수율 29%

시약·촉매·용매 2

HCID 178418476HCID 178418476, 화합물촉매
HCID 31374
Dimethylacetamide
용매

반응 조건

온도
140 °C

실험 절차

Pd(PPh3)2Cl2 (840 mg, 1.2 mmol) and sodium acetate (200 mg, 2.4 mmol) were added to a solution of 6,7-dimethoxy-3,4-dihydronaphthalene (2, 700 mg, 3.7 mmol) and 1-iodo-2-nitrobenzene (925 mg, 3.7 mmol) in dimethylacetamide (50 mL). The mixture was stirred under nitrogen at 140° C. overnight, and then concentrated in vacuo. Ethyl acetate (60 mL) was added to the residue and washed with distilled water (50 mL). The organic layer was separated and passed through a celite bed. The organic layer was then washed with brine, dried (anhydrous Na2SO4) and concentrated in vacuo. The residue was chromatographed to give compound 3 (330 mg) in 29% yield; 1H NMR (CDCl3) d 2.51(2H, t, J=8.1), 2.92(2H, t, J=8.1), 3.87(3H, s), 3.90(3H, s), 6.45(1H, s), 6.67(1H, s), 6.73(1H, s), 7.38˜7.45 (2H, m), 7.54˜7.62(1H, m), 7.88˜7.93(1H, m); 13C NMR d 28.5, 28.5, 56.6, 111.0, 111.7, 124.9, 127.0, 127.1, 128.1, 128:3, 131.3, 133.3, 135.7, 138.7, 147.9, 148.9.

후처리

  1. concentrationconcentrated in vacuo
  2. additionEthyl acetate (60 mL) was added to the residue
  3. washwashed with distilled water (50 mL)
  4. customThe organic layer was separated
  5. washThe organic layer was then washed with brine
  6. dry with materialdried (anhydrous Na2SO4)
  7. concentrationconcentrated in vacuo
  8. customThe residue was chromatographed

출처 및 근거

ORD 기록
ord-360bed0cdf194b48b7a07eaaa8279644
출처 데이터셋
uspto-grants-2004_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06740650B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트