반응 #346173

ord-36c24f6c62de4ceeaa705f3de9047a49

반응 방정식

O
water
Cl.N[C@@H](CS)C(=O)O
cysteine hydrochloride
NC(=O)NCCBr
β-bromoethylurea
O
water
O
water
NC(=O)NCCC[C@H](N)C(O)=S
white product
NC(=O)NCCC[C@H](N)C(O)=S
3-β-ureidoethylthio alanine

반응 조건

온도
50°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도After cooling
  2. 2
    세척After washing with water
  3. 3
    세척is eluted with an ammoniacal solution
  4. 4
    기타The eluate is evaporated to dryness
  5. 5
    기타the residue is crystallized in an aqueous methanol solution

실험 절차

26.25 g of cysteine hydrochloride and 27.83 g of β-bromoethylurea are dissolved in 150 cc of water under nitrogen. A solution of 13.35 g of soda in 30 cc of water is added during a 40 minute period and the mixture is heated for 3 hours at 50° C. After cooling, there is added to the solution, four times its volume of water and the resulting mixture is passed over a cation exchange resin. After washing with water, the product fixed on the resin is eluted with an ammoniacal solution. The eluate is evaporated to dryness and the residue is crystallized in an aqueous methanol solution. There are obtained 19.5 grams of the white product melting at 220° C with decomposition.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04035492uspto-grants-1977_07