Reaktion #966782

ord-b511094160684e6f856a61165f51b79d

Reaktionsgleichung

C[C@@H]1CNCCN1C(=O)OC(C)(C)C
(R)-1-Boc-2-methylpiperazine
CC(=O)O[BH-](OC(C)=O)OC(C)=O.[Na+]
sodium triacetoxyborohydride
CC(C)=O
acetone
CC(=O)O
acetic acid
CC(C)N1CCN(C(=O)OC(C)(C)C)[C@H](C)C1
(R)-1-Boc-2-methyl-4-isopropylpiperazine

Lösungsmittel

Reaktionsbedingungen

Temperatur
60°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Extraktionextracted three times with diethyl ether
  2. 2
    TrocknenThe combined organics were dried over sodium sulfate
  3. 3
    Filtrationfiltered
  4. 4
    Einengenconcentrated
  5. 5
    Sonstigeused without further purification

Vorschrift

To (R)-1-Boc-2-methylpiperazine (200.0 mg, 0.999 mmol) and sodium triacetoxyborohydride (444.5 mg, 2.097 mmol) in DMF (5 mL) was added acetone (116 mg, 0.147 mL, 1.997 mmol) and acetic acid (90.0 mg, 86 μL, 1.498 mmol). The reaction mixture was heated at 60° C. for 1 h. The reaction mixture was diluted with water and extracted three times with diethyl ether. The combined organics were dried over sodium sulfate, filtered, concentrated, and used without further purification. LCMS-ESI+: calc'd for C13H27N2O2 (M+H+): 243.2; Found: 243.1 (M+H+).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08987250B2uspto-grants-2015_03