Guanidine → HCID 178427207、化合物

HRID 597491

反応式

HRID 597491 の反応式
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

参加物

6

反応物 3

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

生成物 1

HCID 178427207HCID 178427207、化合物

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒2 回HCID 5742Guanidine Hydrochloride溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-189416d745004e3c86229c202cd109d6
出典データセット
uspto-grants-1977_03
特許番号
US04014876

関連ノート

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