Water → HCID 86723563, Verbindung

HRID 2201657Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2201657
[CH2:1]=[C:2]1[CH2:5][CH:4]([CH2:6][NH2:7])[CH2:3]1.C([O-])([O-])=O.[Na+].[Na+].Cl[C:15]([O:17][CH2:18][C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)=[O:16].O>O1CCCC1>[CH2:1]=[C:2]1[CH2:5][CH:4]([CH2:6][NH:7][C:15](=[O:16])[O:17][CH2:18][C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[CH2:3]1

Komponenten

6

Edukt 4

HCID 962WaterHCID 10340Sodium CarbonateHCID 10387Benzyl chloroformateHCID 177500821-(3-Methylidenecyclobutyl)methanamine

Produkt 1

HCID 86723563HCID 86723563, VerbindungAusbeute 56,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

Compound 4-2 (3 g, 30.9 mmol) was dissolved in 50 mL of tetrahydrofuran, added Na2CO3 (6.3 g, 60 mmol) and benzyl chloroformate (5.25 g, 30.8 mmol). The mixture was stirred for 12 hours at room temperature, added 100 mL of water, extracted three times with 300 mL of ethyl acetate, combined the organic phases, rotary evaporated to remove solvents and purified by column chromatography (petroleum ether/ethyl acetate=10:1) to give Compound 4-3 (4 g, 56% yield).

Aufarbeitung

  1. extractionextracted three times with 300 mL of ethyl acetate
  2. customrotary evaporated
  3. customto remove solvents
  4. custompurified by column chromatography (petroleum ether/ethyl acetate=10:1)

Quellen und Nachweise

ORD-Eintrag
ord-eef0e8133ab7412380e1dd79abf4ccb8
Quelldatensatz
uspto-grants-2016_06
Patentnummer
US09365499B2

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