تفاعل #76025

ord-b5644432ac1448a9b92abb0f03571ed0

الكواشف

لا شيء

ظروف التفاعل

درجة الحرارة
20°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىAfter concentration of the reaction mass under reduced pressure (5 kPa) at a temperature in the region of 50° C., the oil obtained
  2. 2
    ترشيحThe crystals are filtered off
  3. 3
    أخرىdried under reduced pressure (10 Pa) at a temperature in the region of 60° C

الإجراء التجريبي

The process is performed as in Example 3, starting with 8.1 g of (+)-(2S)-2-amino-3-cyclohexyl-1-propanol and 9.8 cm3 of tert-butyl isothiocyanate in 79 cm3 of ethanol. The reaction medium is stirred for 72 hours at a temperature in the region of 20° C. After concentration of the reaction mass under reduced pressure (5 kPa) at a temperature in the region of 50° C., the oil obtained is taken up in 110 cm3 of cold petroleum ether. The crystals are filtered off and dried under reduced pressure (10 Pa) at a temperature in the region of 60° C. 11.1 g of N-(tert-butyl)-N′-[(1S)-1-cyclohexylmethyl-2-hydroxyethyl]thiourea are obtained in the form of a white solid melting at 97° C.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06699895B2uspto-grants-2004_03