反応 #65346

ord-7aa613c29b004721978c946d018d6d83

溶媒

反応条件

温度
4°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.WAITAfter 3 hrs
  2. 2
    ろ過the suspension was filtered
  3. 3
    その他to remove the first batch of product crystals
  4. 4
    温度the suspension cooled to 4° C
  5. 5
    ろ過The suspension was filtered
  6. 6
    その他to remove the second batch of product crystals

実験手順

2,6-Diamino-9-(2-deoxy-2-fluoro-β-D-ribofuranosyl)-9H-purine (0.20 g, 0.64 mmole), prepared as in Example 6, was dissolved in 15 ml of water. Calf intestinal adenosine deaminase (4 I.U., Boehringer Mannheim) was added and the solution incubated at 37° for 4 days. The solution was cooled to 4° C. After 3 hrs, the suspension was filtered to remove the first batch of product crystals. The volume of the filtrate was reduced under vacuum and the suspension cooled to 4° C. The suspension was filtered to remove the second batch of product crystals. The batches of product crystals were combined, suspended in water and lyophilized to obtain title compound that analyzed as a 1.3 hydrate.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05420115uspto-grants-1995_05