Ammonia → HCID 178485122、化合物

HRID 867164ノート

反応式

HRID 867164 の反応式
[C:1]([NH:3][C:4]([NH:6][CH3:7])=[NH:5])#[N:2].Cl.[NH2:9][C:10]1[CH:14]=[C:13]([CH3:15])[O:12][N:11]=1.N>O>[CH3:7][NH:6][C:4]([NH:3][C:1]([NH:9][C:10]1[CH:14]=[C:13]([CH3:15])[O:12][N:11]=1)=[NH:2])=[NH:5]

参加物

5

反応物 3

HCID 222AmmoniaHCID 203177225-Methylisoxazol-3-amine hydrochlorideHCID 178485119HCID 178485119、化合物

生成物 1

HCID 178485122HCID 178485122、化合物収率 27.6%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

In a reactor are added 4.9 g of 1-cyano-3-methyl-guanidine, 6.7 g of 3-amino-5-methyl-isoxazole hydrochloride and 1.3 ml of water. The reaction mixture is heated until dissolution is complete, after which the reaction is exothermal. After cooling, the reaction mixture is taken up into 30 ml water followed by 3 ml ammonia (d = 0.89). It is then extracted with 30 ml methylene chloride. After drying, treatment with carbon black and evaporation of the solvent, the residue is crystallized from absolute ethanol, to give 2.7 g of 1-methyl-5-(5-methyl-isoxazol-3-yl)-biguanide. M.p. (cap.) = 140° C. followed by resolidification, then 150°-151° C. with introduction at 140° C. and heating at a rate of 2° C./minute.

後処理

  1. temperatureThe reaction mixture is heated until dissolution
  2. temperatureAfter cooling
  3. extractionIt is then extracted with 30 ml methylene chloride
  4. customAfter drying
  5. customtreatment with carbon black and evaporation of the solvent
  6. customthe residue is crystallized from absolute ethanol

出典と根拠

ORDレコード
ord-ecc80cdd1a6e40ca926f4ac2950db676
出典データセット
uspto-grants-1978_07
特許番号
US04103010

反応ノート

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