Guanidine → HCID 178427207, 화합물

HRID 597491

반응식

HRID 597491 반응식
CC[O-].[Na+].[NH2:5][C:6]([NH2:8])=[NH:7].[CH3:9][C:10]1[O:14][N:13]=[C:12]([C:15](OCC)=[O:16])[CH:11]=1>C(O)C.Cl.NC(N)=N>[CH3:9][C:10]1[O:14][N:13]=[C:12]([C:15]([NH:7][C:6]([NH2:8])=[NH:5])=[O:16])[CH:11]=1

참가 물질

6

반응물 3

HCID 3520GuanidineHCID 76677Ethyl 5-methylisoxazole-3-carboxylateHCID 2723922Sodium ethoxide

생성물 1

HCID 178427207HCID 178427207, 화합물

시약·촉매·용매 2

HCID 702Ethanol용매2회HCID 5742Guanidine Hydrochloride용매

실험 절차

To a solution of sodium ethylate (75 parts by weight) in anhydrous ethanol (500 parts by volume), guanidine monohydrochloride (96 parts by weight) is added under stirring and ice-cooling to make an ethanolic solution of free guanidine. To this solution, a solution of ethyl 5-methylisoxazole-3-carboxylate (155 parts by weight) in anhydrous ethanol (200 parts by volume) is added within 2 hours under stirring at 40° C. The resultant mixture is allowed to stand at 20° C for 12 hours. The precipitated crude crystals are filtered off, washed with a small amount of water and recrystallized from ethanol to give 1-(5-methyl-3-isoxazolylcarbonyl)guanidine as colorless prisms melting at 192° to 192.5° C under decomposition. IR (Nujol): 1652 cm-1 (=C=O).

후처리

  1. temperatureice-cooling
  2. stirringunder stirring at 40° C
  3. customThe precipitated crude crystals
  4. filtrationare filtered off
  5. washwashed with a small amount of water
  6. customrecrystallized from ethanol

출처 및 근거

ORD 기록
ord-189416d745004e3c86229c202cd109d6
출처 데이터셋
uspto-grants-1977_03
특허 번호
US04014876

연결된 노트

불러오는 중…