Ammonia → HCID 178485122, 화합물

HRID 867164노트

반응식

HRID 867164 반응식
[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]

참가 물질

5

반응물 3

HCID 222AmmoniaHCID 203177225-Methylisoxazol-3-amine hydrochlorideHCID 178485119HCID 178485119, 화합물

생성물 1

HCID 178485122HCID 178485122, 화합물수율 27.6%

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ecc80cdd1a6e40ca926f4ac2950db676
출처 데이터셋
uspto-grants-1978_07
특허 번호
US04103010

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