Tert-butyl 3-aminoazetidine-1-carboxylate → HCID 58777638, Verbindung

HRID 1371775Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1371775
[NH2:1][C:2]1[C:7]([C:8]([C:10]2[C:15]([O:16][CH3:17])=[CH:14][CH:13]=[C:12]([F:18])[C:11]=2[F:19])=[O:9])=[CH:6][N:5]=[C:4](Cl)[N:3]=1.[C:21]([O:25][C:26]([N:28]1[CH2:31][CH:30]([NH2:32])[CH2:29]1)=[O:27])([CH3:24])([CH3:23])[CH3:22]>C(Cl)Cl.C(O)C>[C:21]([O:25][C:26]([N:28]1[CH2:31][CH:30]([NH:32][C:4]2[N:3]=[C:2]([NH2:1])[C:7]([C:8](=[O:9])[C:10]3[C:15]([O:16][CH3:17])=[CH:14][CH:13]=[C:12]([F:18])[C:11]=3[F:19])=[CH:6][N:5]=2)[CH2:29]1)=[O:27])([CH3:24])([CH3:22])[CH3:23]

Komponenten

5

Edukt 2

HCID 1516507Tert-butyl 3-aminoazetidine-1-carboxylateHCID 21070550HCID 21070550, Verbindung

Produkt 1

HCID 58777638HCID 58777638, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 6344DichloromethaneLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

To a stirred suspension of chloropyrimidine (700 mg, 2.34 mmol, Example 289) in methylene chloride (30 mL), amine (525 mg, 5.64 mmol, Example 318) in ethanol (30 mL) was added and the mixture heated at 80° C. for 4.5 hours. The solvent was removed and the residue was dissolved in ethyl acetate and the mixture was washed successively with 0.5N hydrochloric acid and water. The organic layer was dried with sodium sulfate and concentrated to give a white solid. 1.0 g, 98%. MS (ES) MH+=436.

Aufarbeitung

  1. additionwas added
  2. customThe solvent was removed
  3. dissolutionthe residue was dissolved in ethyl acetate
  4. washthe mixture was washed successively with 0.5N hydrochloric acid and water
  5. dry with materialThe organic layer was dried with sodium sulfate
  6. concentrationconcentrated
  7. customto give a white solid

Quellen und Nachweise

ORD-Eintrag
ord-dd962719fdbd4bd0bc96e9960a153395
Quelldatensatz
uspto-grants-2007_01
Patentnummer
US07157455B2

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