Diisopropylethylamine → HCID 131737175, Verbindung

HRID 61425Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 61425
[C:1]([O:5][C:6]([CH:8]1[CH2:13][CH2:12][CH2:11][NH:10][CH:9]1C(O)=O)=[O:7])([CH3:4])([CH3:3])[CH3:2].[CH:17]([C:20]1[CH:21]=[C:22]([C:26]2[CH2:27][CH2:28]NCC=2)[CH:23]=[CH:24][CH:25]=1)([CH3:19])[CH3:18].C1CN([P+]([O:48]N2N=NC3C=CC=CC2=3)(N2CCCC2)N2CCCC2)CC1.F[P-](F)(F)(F)(F)F.[CH:65]([N:68]([CH:71](C)C)CC)(C)[CH3:66]>CN(C=O)C.CCOC(C)=O>[C:1]([O:5][C:6]([CH:8]1[CH:13]([C:71]([N:68]2[CH2:65][CH:66]=[CH:28][CH2:27][CH:26]2[C:22]2[CH:23]=[CH:24][CH:25]=[C:20]([CH:17]([CH3:18])[CH3:19])[CH:21]=2)=[O:48])[CH2:12][CH2:11][NH:10][CH2:9]1)=[O:7])([CH3:2])([CH3:3])[CH3:4]

Komponenten

7

Edukt 4

HCID 81531DiisopropylethylamineHCID 2724699PyBOPHCID 22956954HCID 22956954, VerbindungHCID 673051604-(3-Isopropyl-phenyl)-1,2,3,6-tetrahydro-pyridine

Produkt 1

HCID 131737175HCID 131737175, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6228DimethylformamideLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

To a 0° C. solution of piperidine-2,3-dicarboxylic acid 3-tert-butyl ester (100 mg) in DMF (0.6 mL) was added sequentially, 4-(3-isopropyl-phenyl)-1,2,3,6-tetrahydropyridine (97 mg). PyBOP (232 mg), and diisopropylethylamine (0.152 mL). The resultant mixture was stirred at rt overnight. The reaction solution was diluted with EtOAc and washed with saturated NaHCO3 solution (×3), water, and brine. The organic layers were dried over MgSO4, filtered, and concentrated to dry under reduced pressure. The residue was used in next step without further purifications. MS (ESI): 413.2 (M+H+)

Aufarbeitung

  1. washwashed with saturated NaHCO3 solution (×3), water, and brine
  2. dry with materialThe organic layers were dried over MgSO4
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customto dry under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-b9786a318b304490bf004bef6f1818a3
Quelldatensatz
uspto-grants-2016_09
Patentnummer
US09440958B2

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