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HCID 58442810, 화합물 → HCID 58442811, 화합물

HRID 41627
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HRID 41627 반응식
[CH3:1][O:2][C:3]([C:5]1[C:6]([C:11]2[CH2:12][CH2:13][N:14]([C:17]([O:19][C:20]([CH3:23])([CH3:22])[CH3:21])=[O:18])[CH2:15][CH:16]=2)=[N:7][CH:8]=[CH:9][CH:10]=1)=[O:4].[H][H]>[OH-].[OH-].[Pd+2].CCOC(C)=O>[CH3:1][O:2][C:3]([C:5]1[C:6]([CH:11]2[CH2:12][CH2:13][N:14]([C:17]([O:19][C:20]([CH3:23])([CH3:22])[CH3:21])=[O:18])[CH2:15][CH2:16]2)=[N:7][CH:8]=[CH:9][CH:10]=1)=[O:4]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 58442810HCID 58442810, 화합물HCID 178418361HCID 178418361, 화합물

생성물 1

HCID 58442811HCID 58442811, 화합물수율 59.5%

시약·촉매·용매 2

HCID 9942167Palladium hydroxide촉매HCID 8857Ethyl Acetate용매

실험 절차

Pd(OH)2/C (690 mg) was added to a solution of 3′,6′-dihydro-2′H-[2,4]bipyridinyl-3,1′-dicarboxylic acid 1′-t-butyl ester 3-methyl ester (2.0 g, 6.3 mmol, 1.0 eq.) in PE (220 mL) and EtOAc (50 mL). Hydrogen gas (1 atm) was introduced into the reaction vessel, and the solution was stirred for 20 hours at room temperature. The reaction mixture was filtered and the remaining mixture was concentrated under vacuum. The residue was applied onto a silica gel column and eluted with EtOAc/PE (1:8) to yield 3′,4′,5′,6′-tetrahydro-2′H-[2,4]bipyridinyl-3,1′-dicarboxylic acid 1′-t-butyl ester 3-methyl ester (1.2 g) as a colorless oil.

후처리

  1. filtrationThe reaction mixture was filtered
  2. concentrationthe remaining mixture was concentrated under vacuum
  3. washeluted with EtOAc/PE (1:8)

출처 및 근거

ORD 기록
ord-67c3c583cbd4498ea95d504ee0646e9b
출처 데이터셋
uspto-grants-2013_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08530663B2

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