Dichloromethane methanol → 4-Cyclopropylpyridin-3-amine

HRID 705360Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 705360
[CH:1]1([C:4]2[CH:9]=[CH:8][N:7]=[CH:6][C:5]=2[NH:10]C(=O)OC(C)(C)C)[CH2:3][CH2:2]1.CO.C(Cl)Cl>Cl.O1CCOCC1>[CH:1]1([C:4]2[CH:9]=[CH:8][N:7]=[CH:6][C:5]=2[NH2:10])[CH2:3][CH2:2]1

Komponenten

5

Edukt 2

HCID 21226129Dichloromethane methanolHCID 67981637Tert-butyl 4-cyclopropylpyridin-3-ylcarbamate

Produkt 1

HCID 668019694-Cyclopropylpyridin-3-amineAusbeute 144,4 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 313Hydrochloric AcidLösungsmittelHCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

Tert-butyl 4-cyclopropylpyridin-3-ylcarbamate (393 mg, 1.677 mmol) was dissolved in 4 M HCl in dioxane (30 mL), and stirred at room temperature for 1 hour, the reaction rapidly becoming a white heterogeneous mixture. TLC (SiO2, 5% methanol/CH2Cl2) showed reaction complete after 1 hour. The solvent was removed by rotary evaporation, the residue was triturated with diethyl ether and vacuum filtered to collect the solid, and the solid was dried in a vacuum oven at 50° C. for 1 hour to afford the product as a beige solid (325 mg).

Aufarbeitung

  1. customthe reaction
  2. customreaction complete after 1 hour
  3. customThe solvent was removed by rotary evaporation
  4. customthe residue was triturated with diethyl ether and vacuum
  5. filtrationfiltered
  6. customto collect the solid
  7. customthe solid was dried in a vacuum oven at 50° C. for 1 hour

Quellen und Nachweise

ORD-Eintrag
ord-35f586d1acbf46cd81d8712eaa622790
Quelldatensatz
uspto-grants-2015_11
Patentnummer
US09173887B2

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