تفاعل #47029

ord-a77ac20d78574144af2dbf10417d08bd

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىevaporated to dryness
  2. 2
    ترشيحThe insoluble material is filtered

الإجراء التجريبي

A mixture of intermediate 25 (200 mg, 0.786 mmol) and 2,4-dichlorobenzyl chloride (0.218 mL, 1.57 mmol) in abs. EtOH (2 mL) is heated at 95° C. for 24 h. The reaction mixture is cooled to RT, evaporated to dryness, and the residue suspended in Et2O. The insoluble material is filtered to give 287 mg of the product 199. 1H NMR (DMSO-d6) δ 11.38 (s, 2 H), 7.95-7.75 (m, 2 H), 7.65-7.50 (m, 1 H), 7.20-7.00 (m, 6 H), 7.00-6.80 (m, 4 H), 5.83 (s, 2 H), 4.90 (s, 2 H); MS: m/z 413 (M++1).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07741493B2uspto-grants-2010_06