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

Water → 4-(4-tert-butylphenyl)-2-methyl-3,5,6,7-tetrahydro-s-indacen-1(2H)-one

HRID 271792
노트
인쇄 미리보기

반응식

HRID 271792 반응식
Br[C:2]1[C:13]2[CH2:12][CH2:11][CH2:10][C:9]=2[CH:8]=[C:7]2[C:3]=1[CH2:4][CH:5]([CH3:15])[C:6]2=[O:14].C(OB([C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1)O)(C)(C)C.C(=O)([O-])[O-].[Na+].[Na+].O>C(COC)OC.C([O-])(=O)C.[Pd+2].C([O-])(=O)C.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>[C:3]([C:23]1[CH:24]=[CH:25][C:26]([C:2]2[C:13]3[CH2:12][CH2:11][CH2:10][C:9]=3[CH:8]=[C:7]3[C:3]=2[CH2:4][CH:5]([CH3:15])[C:6]3=[O:14])=[CH:27][CH:28]=1)([CH3:7])([CH3:4])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 962Water2회HCID 10340Sodium CarbonateHCID 235470494-Bromo-2-methyl-2,3,6,7-tetrahydro-s-indacen-1(5H)-oneHCID 66584345Tert-butylphenylboronic acid

생성물 1

HCID 687458344-(4-tert-butylphenyl)-2-methyl-3,5,6,7-tetrahydro-s-indacen-1(2H)-one수율 139.6%

시약·촉매·용매 3

HCID 11776
Triphenylphosphine
촉매
HCID 167845palladium(II) acetate촉매
HCID 80711,2-Dimethoxyethane용매

실험 절차

0.3 g of palladium acetate (3 mol %) and 0.7 g of triphenylphosphine (6 mol %) were added to a well-stirred mixture of 12 g (0.045 mol) of 4-bromo-2-methyl-3,5,6,7-tetrahydro-s-indacen-1(2H)-one (1b), 11.2 g (0.063 mol) of tert-butylphenylboronic acid and 13.4 g (0.126 mol) of sodium carbonate in 170 ml of dimethoxyethane (DME)/56 ml of water. The reaction mixture was refluxed for 6 hours, poured into water and extracted with methylene chloride (5×100 ml). The combined organic phases were washed with sodium carbonate solution and water and dried over magnesium sulfate. After removal of the solvent, the crude product was chromatographed on silica gel (hexane/chloroform from 4/1 to 1/1). This gave 10 g (70% yield) of the compound (1c) as a viscous oil.

후처리

  1. temperatureThe reaction mixture was refluxed for 6 hours
  2. extractionextracted with methylene chloride (5×100 ml)
  3. washThe combined organic phases were washed with sodium carbonate solution and water
  4. dry with materialdried over magnesium sulfate
  5. customAfter removal of the solvent
  6. customthe crude product was chromatographed on silica gel (hexane/chloroform from 4/1 to 1/1)

출처 및 근거

ORD 기록
ord-6fb62cb35617479281ac8ec352db1097
출처 데이터셋
uspto-grants-2008_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07452949B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트