反应 #9229

ord-b034843c1eae49b58ee346d1b1960c87

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他was purged with nitrogen gas
  2. 2
    其他by bubbling of hydrogen gas
  3. 3
    过滤filtered
  4. 4
    浓缩concentrated
  5. 5
    其他purified by preparative TLC

实验过程

A suspension of 1-(6-phenylacetylenyl-2-benzothiazolyl)-3-ethylurea (0.032 g, 83% purity by weight, 0.083 mmol) and Lindlar catalyst (0.030 g, 5% weight purity, 0.012 mmol, 0.15 eq) in 2 mL ethanol was purged with nitrogen gas, followed by bubbling of hydrogen gas. It was stirred under hydrogen atmosphere for about 36 hours. The mixture was taken up in 10 mL MeOH, filtered, concentrated, and purified by preparative TLC to give 0.011 g (41%) of the desired compound. LC/MS 324 (M+1); LC retention time 2.84 min.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07091227B2uspto-grants-2006_08