反応 #1005984

ord-1fc12bf65f814bf28a0763330ed57e9f

反応方程式

CN(CCCCN=[N+]=[N-])C(=O)n1cnc(-c2ccccc2)c1
compound 48
CN(CCCCN=[N+]=[N-])C(=O)n1cnc(-c2ccccc2)c1
N-(4-azidobutyl)-N-methyl-4-phenyl-1H-imidazole-1-carboxamide
c1ccc(P(c2ccccc2)c2ccccc2)cc1
triphenylphosphine
S=C=S
Carbondisulfide
CN(CCCCN=C=S)C(=O)n1cnc(-c2ccccc2)c1
crude compound
CN(CCCCN=C=S)C(=O)n1cnc(-c2ccccc2)c1
N-(4-isothiocyanatobutyl)-N-methyl-4-phenyl-1H-imidazole-1-carboxamide

溶媒

反応条件

温度
50°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.WAITthe stirring continued at 50° C. for 4 h
  2. 2
    その他Reaction
  3. 3
    温度was cooled to r.t.
  4. 4
    その他solvent was evaporated on Rotavapor

実験手順

To a compound 48 (0.85 mmol) in anhydrous toluene (20 mL) was added triphenylphosphine (1 mmol) and reaction mixture was stirred at 50° C. for 2 h. Carbondisulfide (10 mmol) was added and the stirring continued at 50° C. for 4 h. Reaction was cooled to r.t. and solvent was evaporated on Rotavapor to give a crude compound which on purification by Biotage SP1 gave a pure isothiocyante 49.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US09271962B2uspto-grants-2016_03