Reaktion #61070

ord-617ef31056a84a9fb21cf436620f582e

Reaktionsgleichung

ClCCl.O
water CH2Cl2
Brc1cc[nH]n1
3-bromo-pyrazole
ClC(c1ccccc1)(c1ccccc1)c1ccccc1
triphenylmethyl chloride
CCN(CC)CC
Et3N
Brc1ccn(C(c2ccccc2)(c2ccccc2)c2ccccc2)n1
title compound
Ausbeute 64.0%
Brc1ccn(C(c2ccccc2)(c2ccccc2)c2ccccc2)n1
3-Bromo-1-(triphenylmethyl)-1H-pyrazole
Ausbeute 64.0%

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe phases were separated
  2. 2
    Extraktionthe aqueous layer was further extracted with CH2Cl2 (2×30 mL)
  3. 3
    TrocknenThe combined organic extracts were dried over anh. Na2SO4
  4. 4
    Filtrationthe solids were filtered
  5. 5
    Sonstigethe solvent evaporated
  6. 6
    SonstigeThe residue was purified by flash chromatography (silica gel, 100% CH2Cl2)

Vorschrift

To a solution of 3-bromo-pyrazole (2.0 g, 13.6 mmol) in anh. CH2Cl2 (40 mL), at r.t., under N2, were added triphenylmethyl chloride (4.17 g, 1.1 eq) and Et3N (2.1 mL, 1.1 eq). The reaction mixture was stirred at r.t. for 4 hr. It was poured into water/CH2Cl2. The phases were separated and the aqueous layer was further extracted with CH2Cl2 (2×30 mL). The combined organic extracts were dried over anh. Na2SO4, the solids were filtered and the solvent evaporated. The residue was purified by flash chromatography (silica gel, 100% CH2Cl2) to give the title compound as a white solid (3.39 g, 64%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07427630B2uspto-grants-2008_09