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(4-Methoxy-3-methylphenyl)boronic acid → [4-(4-Methoxy-3-methyl-benzoyl)-piperidin-1-yl]-acetic acid ethyl ester

HRID 713445
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HRID 713445 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6](B(O)O)=[CH:5][C:4]=1[CH3:12].[CH2:13]([O:15][C:16](=[O:33])[CH2:17][N:18]1[CH2:23][CH2:22][CH:21]([C:24](SC2C=CC=CC=2)=[O:25])[CH2:20][CH2:19]1)[CH3:14]>COCCOC.C(OCC)(=O)C.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].S1C=CC=C1C([O-])=O.[Cu+]>[CH2:13]([O:15][C:16](=[O:33])[CH2:17][N:18]1[CH2:23][CH2:22][CH:21]([C:24](=[O:25])[C:6]2[CH:7]=[CH:8][C:3]([O:2][CH3:1])=[C:4]([CH3:12])[CH:5]=2)[CH2:20][CH2:19]1)[CH3:14]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 2

HCID 2773487(4-Methoxy-3-methylphenyl)boronic acidHCID 89389237(4-Phenylsulfanylcarbonyl-piperidin-1-yl)-acetic acid ethyl ester

생성물 1

HCID 71226501[4-(4-Methoxy-3-methyl-benzoyl)-piperidin-1-yl]-acetic acid ethyl ester수율 46.2%

시약·촉매·용매 4

HCID 9811564Bis(dibenzylideneacetone)palladium촉매
HCID 11194830
Cuprous 2-thiophenecarboxylate
촉매
HCID 80711,2-Dimethoxyethane용매
HCID 8857Ethyl Acetate용매

실험 절차

To a mixture of 4-methoxy-3-methyl phenylboronic acid (0.32 g, 1.95 mmol), ligand TFP (0.06 g, 0.26 mmol), Pd2dba3 (0.12 g, 0.13 mmol), copper (I) thiophene-2-carboxylate (0.37 g, 2.0 mmol) was added a solution of (4-phenylsulfanylcarbonyl-piperidin-1-yl)-acetic acid ethyl ester (0.4 g, 1.3 mmol) in 6 mL of DME. It was stirred at RT for 16 hours, the reaction mixture was diluted with ethyl acetate, filtered through celite then concentrated in vacuo. Purification by flash chromatography gave the title compound (0.2 g, 0.6 mmol). MS (ESI) m/z 319.8 (M+H+); HPLC (Novapak 150×3.9 mm C-18 column: mobile phase: 35-90% acetonitrile/water with 0.1% TFA, at 2 mL/min over 2 min.) t 1.36 min.

후처리

  1. filtrationfiltered through celite
  2. concentrationthen concentrated in vacuo
  3. customPurification by flash chromatography

출처 및 근거

ORD 기록
ord-095f9cee8b4c400db75416dcf43a063c
출처 데이터셋
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09181266B2

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