تفاعل #66513

ord-aefa367428334f35889df964d4cf7e2b

معادلة التفاعل

Ic1cn[nH]c1
4-iodo-1H-pyrazole
COc1ccc(CCl)cc1
1-(chloromethyl)-4-methoxybenzene
O=C([O-])[O-].[K+].[K+]
K2CO3
COc1ccc(Cn2cc(I)cn2)cc1
4-iodo-1-(4-methoxybenzyl)-1H-pyrazole
المردود 88.2%

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
60°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةThe reaction mixture was cooled to room temperature
  2. 2
    ترشيحwas filtered
  3. 3
    تركيزThe filtrate was concentrated under reduced pressure
  4. 4
    أخرىThe crude product was purified by flash chromatography over silica gel

الإجراء التجريبي

According to Scheme 6 Step 1: A suspension of 4-iodo-1H-pyrazole (26.3 mmol, 5.11 g), 1-(chloromethyl)-4-methoxybenzene (29.0 mmol, 3.95 mL) and K2CO3 (39.5 mmol, 5.46 g) in acetonitrile (150 mL) was heated at 60° C. overnight. The reaction mixture was cooled to room temperature and was filtered. The filtrate was concentrated under reduced pressure. The crude product was purified by flash chromatography over silica gel using DCM as eluent to afford 4-iodo-1-(4-methoxybenzyl)-1H-pyrazole (23.2 mmol, 7.3 g, 88%) as a yellow solid.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08524718B2uspto-grants-2013_09