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

Tetrahydrofuran → 2-[5-(4-{1-[4-(t-Butyl-dimethyl-silanyloxy)-3-methyl-phenyl]-1-ethyl-propyl}-2-methyl-phenyl)-furan-2-yl]-propan-2-ol

HRID 546836
노트
인쇄 미리보기

반응식

HRID 546836 반응식
[CH3:1][Mg]Br.COC(C1OC([C:13]2[CH:18]=[CH:17][C:16]([C:19]([C:24]3[CH:29]=[CH:28][C:27]([O:30][Si:31]([C:34]([CH3:37])([CH3:36])[CH3:35])([CH3:33])[CH3:32])=[C:26]([CH3:38])[CH:25]=3)([CH2:22][CH3:23])[CH2:20][CH3:21])=[CH:15][C:14]=2[CH3:39])=CC=1)=O.C([O:43][CH2:44][CH3:45])(=O)C.[O:46]1[CH2:50][CH2:49][CH2:48][CH2:47]1>>[C:34]([Si:31]([CH3:32])([CH3:33])[O:30][C:27]1[CH:28]=[CH:29][C:24]([C:19]([C:16]2[CH:17]=[CH:18][C:13]([C:50]3[O:46][C:47]([C:44]([OH:43])([CH3:45])[CH3:1])=[CH:48][CH:49]=3)=[C:14]([CH3:39])[CH:15]=2)([CH2:20][CH3:21])[CH2:22][CH3:23])=[CH:25][C:26]=1[CH3:38])([CH3:37])([CH3:36])[CH3:35]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 4

HCID 8028Tetrahydrofuran2회HCID 8857Ethyl AcetateHCID 57709087HCID 57709087, 화합물HCID 178418573HCID 178418573, 화합물

생성물 1

HCID 670651812-[5-(4-{1-[4-(t-Butyl-dimethyl-silanyloxy)-3-methyl-phenyl]-1-ethyl-propyl}-2-methyl-phenyl)-furan-2-yl]-propan-2-ol

실험 절차

A 3 M solution of methylmagnesium bromide in tetrahydrofuran (0.08 mL, 0.24 mmol) was added to a solution of 5-(4-{1-[4-(t-butyl-dimethyl-silanyloxy)-3-methyl-phenyl]-1-ethyl-propyl}-2-methyl-phenyl)-furan-2-carboxylic acid methyl ester (Example 19-(2); 20 mg, 0.039 mmol) in tetrahydrofuran (0.2 mL) at 0° C., and the mixture was stirred at the same temperature for three hours. Ethyl acetate was added to the reaction solution. The organic layer was washed with a sodium bisulfate aqueous solution and brine and dried over anhydrous magnesium sulfate. Then, the solvent was distilled off under reduced pressure to give crude 2-[5-(4-{1-[4-(t-butyl-dimethyl-silanyloxy)-3-methyl-phenyl]-1-ethyl-propyl}-2-methyl-phenyl)-furan-2-yl]-propan-2-ol (8.5 mg). A 1 M solution of tetrabutylammonium fluoride in tetrahydrofuran (0.03 mL, 0.03 mmol) was added to a solution of the resulting compound in tetrahydrofuran (0.2 mL), and the mixture was stirred at room temperature for one minute. Ethyl acetate was added to the reaction mixture. The organic layer was washed with distilled water and brine and then dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. (R)-(−)-Dihydro-5-(p-tolyl-sulfonyloxymethyl)-2(3H)-furanone (11 mg, 0.041 mmol) and potassium carbonate (9 mg, 0.066 mmol) were added to a solution of the residue (6.5 mg) in N,N-dimethylformamide (0.2 mL) at room temperature, and the mixture was stirred at room temperature for 11 hours. Ethyl acetate was added to the reaction solution. The organic layer was washed with brine and dried over anhydrous magnesium sulfate, and then the solvent was distilled off under reduced pressure. The residue was purified by silica gel chromatography (n-hexane/ethyl acetate=1/1) to give the title compound (2.8 mg, 34.5%).

후처리

  1. washThe organic layer was washed with a sodium bisulfate aqueous solution and brine
  2. dry with materialdried over anhydrous magnesium sulfate
  3. distillationThen, the solvent was distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-72b911fe10b744488363c52ca9b8cc43
출처 데이터셋
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07935688B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트