反応 #2283643

ord-5cb3a0da2b544d7b9ff2ec2c9d6dc9b4

試薬

なし

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度The mixture is heated
  2. 2
    温度to reflux for 3 to 4 hours
  3. 3
    その他The reaction mixture is evaporated
  4. 4
    workup.ADDITION20 ml of ethanol are added
  5. 5
    その他evaporated as well
  6. 6
    workup.ADDITIONAfter that, 10 ml of methanol and 30 ml of acetone are added
  7. 7
    ろ過The crystalline material is filtered
  8. 8
    その他the product is dried under high vacuum overnight

実験手順

The 5-chloropentanenitrile (5.68 g, 48.3 mmol) and thiourea (4.04 g, 53.1 mmol) are mixed in 40 ml of water. The mixture is heated to reflux for 3 to 4 hours. The reaction mixture is evaporated and 20 ml of ethanol are added and then evaporated as well. This is repeated three times. After that, 10 ml of methanol and 30 ml of acetone are added and the mixture is stirred for one hour. The crystalline material is filtered and the product is dried under high vacuum overnight to yield S-(4-cyanobutyl)isothiourea hydrochloride.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08338454B2uspto-grants-2012_12