تفاعل #367108

ord-0dd8cedb2cb44f4cb56ff4b974d81c4e

المذيبات

ظروف التفاعل

درجة الحرارة
4°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةcooled
  2. 2
    ترشيحfiltered
  3. 3
    ترشيحThis mixture was then filtered
  4. 4
    workup.ADDITIONthe filtrate was treated with activated charcoal
  5. 5
    أخرىgiving a green solution
  6. 6
    أخرىthe resulting solid collected
  7. 7
    workup.STIRRINGA 100 mg portion of this solid was stirred with 15 ml of hot water
  8. 8
    ترشيحfiltered through diatomaceous earth
  9. 9
    درجة الحرارةThe filtrate was cooled
  10. 10
    أخرىgiving a solid which
  11. 11
    أخرىwas collected

الإجراء التجريبي

A solution of 20 g of glucosamine hydrochloride, 20 ml of glacial acetic acid, 80 ml of water and 9.1 ml of phenylhydrazine was heated on a steam bath for one hour, then cooled and filtered. The filtrate was hydrogenated in a Parr apparatus with Raney nickel catalyst until the uptake of hydrogen ceased. This mixture was then filtered, the filtrate was treated with activated charcoal and refiltered through diatomaceous earth, giving a green solution. A 6.31 ml portion of this green solution was treated with 0.24 g of sodium bicarbonate and a suspension of 1.66 g of potassium tetrachloroplatinate in 8 ml of water. The resulting reddish brown solution was stirred overnight, then cooled to 4° C. for 3 hours and the resulting solid collected. A 100 mg portion of this solid was stirred with 15 ml of hot water and then filtered through diatomaceous earth. The filtrate was cooled giving a solid which was collected, giving 90 mg of 1,2-diamino-1,2-dideoxy-D-glucitol, compound with platinum chloride (1:1) as yellow grains, mp 265° C. (dec.).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04587331uspto-grants-1986_05