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Sodium Carbonate → HCID 58442808, 화합물

HRID 41635
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HRID 41635 반응식
[CH3:1][O:2][C:3]([C:5]1[CH:9]=[CH:8][O:7][C:6]=1Br)=[O:4].[C:11]([O:15][C:16]([N:18]1[CH2:23][CH:22]=[C:21](B2OC(C)(C)C(C)(C)O2)[CH2:20][CH2:19]1)=[O:17])([CH3:14])([CH3:13])[CH3:12].C([O-])([O-])=O.[Na+].[Na+]>Cl[Pd](Cl)([P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.C1COCC1>[C:11]([O:15][C:16]([N:18]1[CH2:19][CH:20]=[C:21]([C:6]2[O:7][CH:8]=[CH:9][C:5]=2[C:3]([O:2][CH3:1])=[O:4])[CH2:22][CH2:23]1)=[O:17])([CH3:14])([CH3:12])[CH3:13]
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참가 물질

6

반응물 3

HCID 10340Sodium CarbonateHCID 4642098Tert-butyl 4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1,2,3,6-tetrahydropyridine-1-carboxylateHCID 10845885Methyl 2-bromofuran-3-carboxylate

생성물 1

HCID 58442808HCID 58442808, 화합물수율 75.9%

시약·촉매·용매 2

HCID 178418476HCID 178418476, 화합물촉매
HCID 8028Tetrahydrofuran용매

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온도
80 °C

실험 절차

2-Bromofuran-3-carboxylic acid methyl ester (3.0 g, 15 mmol, 1.0 eq.), 4-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)-3,6-dihydro-2H-pyridine-1-carboxylic acid t-butyl ester (4.5 g, 15 mmol, 1.0 eq.), THF (150 mL) and Na2CO3 (30 mL, 60 mmol, 4.0 eq.) were combined. The mixture was degassed and purged with nitrogen (3×). PdCl2(PPh3)2 (0.3 g, 0.4 mmol, 0.03 eq.) was added, and the mixture was again degassed and purged with nitrogen (3×), then heated at 80° C. overnight. The mixture was then cooled and the layers were separated. The THF layer was diluted with EtOAc (150 mL), washed with saturated aqueous NaCl (80 mL) and dried over Na2SO4. The material was filtered and applied onto a silica gel column and purified by chromatography with PE/EtOAc (20:1 to 10:1) to yield 4-(3-methoxycarbonylfuran-2-yl)-3,6-dihydro-2H-pyridine-1-carboxylic acid t-butyl ester (3.5 g) as a white solid.

후처리

  1. customThe mixture was degassed
  2. custompurged with nitrogen (3×)
  3. customthe mixture was again degassed
  4. custompurged with nitrogen (3×)
  5. temperatureThe mixture was then cooled
  6. customthe layers were separated
  7. additionThe THF layer was diluted with EtOAc (150 mL)
  8. washwashed with saturated aqueous NaCl (80 mL)
  9. dry with materialdried over Na2SO4
  10. filtrationThe material was filtered
  11. custompurified by chromatography with PE/EtOAc (20:1 to 10:1)

출처 및 근거

ORD 기록
ord-ec15a4a9acee4949b613c9b22b64e48a
출처 데이터셋
uspto-grants-2013_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08530663B2

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