반응 #8693

ord-2f674e412cd94d6e9616d8a0d73b8925

반응 방정식

Cc1ccc(-c2c(Cl)nc(-c3ccncc3)nc2NS(=O)(=O)CCc2ccccc2)cc1
2-Phenyl-ethanesulfonic acid (6-chloro-2-pyridin-4-yl-5-p-tolyl-pyrimidin-4-yl)-amide
O=C(O)CC(O)(CC(=O)O)C(=O)O
citric acid
Cc1ccc(-c2c(NS(=O)(=O)CCc3ccccc3)nc(-c3ccncc3)nc2OCCO)cc1
2-phenyl-ethanesulfonic acid [6-(2-hydroxy-ethoxy)-2-pyridin-4-yl-5-p-tolyl-pyrimidin-4-yl]-amide

반응 조건

온도
11°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The resulting precipitate was collected
  2. 2
    세척washed with water and diethyl ether
  3. 3
    기타dried

실험 절차

2-Phenyl-ethanesulfonic acid (6-chloro-2-pyridin-4-yl-5-p-tolyl-pyrimidin-4-yl)-amide (480 mg) was added to a solution of K-tert. butylate (580 mg) in ethylene glycol (5 ml). The mixture was stirred at 11° C. for 72 h before it was diluted with water (100 ml), acidified with 10% aq. citric acid (13 ml). The resulting precipitate was collected, washed with water and diethyl ether and dried to give 2-phenyl-ethanesulfonic acid [6-(2-hydroxy-ethoxy)-2-pyridin-4-yl-5-p-tolyl-pyrimidin-4-yl]-amide as a beige powder. LC-MS: tR=4.17 min, [M+1]+=491.24, [M−1]−=489.08.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07091201B2uspto-grants-2006_08