تفاعل #1009892

ord-01fa24a65bfc4cde93e522f09e0bf815

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
84.5°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةto cool to 60° C.
  2. 2
    workup.STIRRINGthe mixture was stirred at 25 to 40° C. for 15 hr
  3. 3
    ترشيحThe crystals were collected by filtration
  4. 4
    غسيلwashed twice with water (100 mL)
  5. 5
    أخرىvacuum-dried (50° C.) to a constant amount

الإجراء التجريبي

To glucosamine hydrochloride (200 g, 0.928 mol) were added water (300 mL) and ammonium thiocyanate (212 g, 2.78 mol, 3.0 equivalents) at 25° C., and the mixture was stirred at 80 to 89° C. for 8 hr. The reaction mixture was allowed to cool to 60° C., water (300 mL) and seed crystals were added thereto, and the mixture was stirred at 25 to 40° C. for 15 hr. The crystals were collected by filtration, washed twice with water (100 mL), and vacuum-dried (50° C.) to a constant amount to give (1R,2S,3R)-1-(2-sulfanyl-1H-imidazol-4-yl)butane-1,2,3,4-tetraol (101.4 g). yield 50%.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US09278938B2uspto-grants-2016_03