反応 #53790

ord-2c8f5600ae6f41b9984d67f20d309d62

反応方程式

CCOP(=O)(Cc1ccc(N)cc1)OCC
diethyl 4-aminobenzylphosphonate
O=C([O-])O.[Na+]
sodium bicarbonate
O
water
S=C(Cl)Cl
Thiophosgene
CCOP(=O)(Cc1ccc(N=C=S)cc1)OCC
isothiocyanate
CCOP(=O)(Cc1ccc(N=C=S)cc1)OCC
Diethyl 4-isothiocyanatobenzylphosphonate

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他The organic and aqueous layers were separated
  2. 2
    乾燥the organic layer dried over magnesium sulfate
  3. 3
    ろ過filtered
  4. 4
    濃縮concentrated

実験手順

Thiophosgene (4.1 mL, 54 mmol) was added al at once to a mixture of diethyl 4-aminobenzylphosphonate (12.04 g, 50 mmol), sodium bicarbonate (8.33 g, 99 mmol), water (100 mL), and dichloromethane (250 mL), and the mixture was stirred at room temperature for about 2 hours. The organic and aqueous layers were separated, the organic layer dried over magnesium sulfate, filtered, and concentrated to give the product isothiocyanate as a brown oil. This was used directly in the next step.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06858739B2uspto-grants-2005_02