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(4-Ethoxy-3-fluorophenyl)boronic acid → 1,1-Dimethylethyl 4-(4-ethoxy-3-fluorobenzoyl)-1-piperidinecarboxylate

HRID 713461
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HRID 713461 반응식
[CH2:1]([O:3][C:4]1[CH:9]=[CH:8][C:7](B(O)O)=[CH:6][C:5]=1[F:13])[CH3:2].[C:14]([O:18][C:19]([N:21]1[CH2:26][CH2:25][CH:24]([C:27](SC2C=CC=CC=2)=[O:28])[CH2:23][CH2:22]1)=[O:20])([CH3:17])([CH3:16])[CH3:15]>C1COCC1.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+]>[C:14]([O:18][C:19]([N:21]1[CH2:26][CH2:25][CH:24]([C:27](=[O:28])[C:7]2[CH:8]=[CH:9][C:4]([O:3][CH2:1][CH3:2])=[C:5]([F:13])[CH:6]=2)[CH2:23][CH2:22]1)=[O:20])([CH3:17])([CH3:16])[CH3:15]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 2

HCID 2782821(4-Ethoxy-3-fluorophenyl)boronic acidHCID 893758004-Phenylsulfanylcarbonyl-piperidine-1-carboxylic acid tert-butyl ester

생성물 1

HCID 712267821,1-Dimethylethyl 4-(4-ethoxy-3-fluorobenzoyl)-1-piperidinecarboxylate수율 82.6%

시약·촉매·용매 3

HCID 9811564Bis(dibenzylideneacetone)palladium촉매
HCID 11194830
Cuprous 2-thiophenecarboxylate
촉매
HCID 8028Tetrahydrofuran용매

실험 절차

To a mixture of 4-ethoxy-3-fluorophenylboronic acid (0.86 g, 4.67 mmol), ligand TFP (0.144 g, 0.62 mmol), Pd2dba3 (0.29 g, 0.31 mmol), copper (I) thiophene-2-carboxylate (0.89 g, 4.7 mmol) was added a solution of 4-phenylsulfanylcarbonyl-piperidine-1-carboxylic acid tert-butyl ester (1.0 g, 3.11 mmol) in 10 mL of THF while purging with N2 at 50° C. After 18 hours the reaction mixture was diluted with ethyl acetate, filtered through celite then concentrated in vacuo. Purification by flash chromatography gave the title compound (0.95 g, 2.57 mmol). MS (ESI) m/z 352.0 (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 1.42 min.

후처리

  1. customwhile purging with N2 at 50° C
  2. additionAfter 18 hours the reaction mixture was diluted with ethyl acetate
  3. filtrationfiltered through celite
  4. concentrationthen concentrated in vacuo
  5. customPurification by flash chromatography

출처 및 근거

ORD 기록
ord-d0bd7f4aa1404a8b81ccc81c987bd368
출처 데이터셋
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09181266B2

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