Реакция #47002

ord-2d62f557fbb243ceaea737eaf4f4f398

Растворители

Условия реакции

Температура
115°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ТемператураThe reaction mixture is cooled to rt
  2. 2
    Температураis heated at 115° C. overnight
  3. 3
    ТемператураThe reaction mixture is cooled to rt
  4. 4
    Другоеthe product is precipitated by the addition of addition of water

Методика

A solution of intermediate 59 (1.0 g, 2.71 mmol) in ethylene glycol (10 mL) is saturated with ammonia and is heated in a pressure tube at 115° C. for 3 h. The reaction mixture is cooled to rt, and saturated with ammonia, and heated is heated at 115° C. overnight. The reaction mixture is cooled to rt, and the product is precipitated by the addition of addition of water to give 226 mg of the product 122. 1H NMR (DMSO-d6) δ 7.10-6.80 (m, 10 H), 6.40 (bs, 3 H), 5.10 (s, 2 H); LC/MS: 2.89 min, m/z 238 (M++1).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07741493B2uspto-grants-2010_06