5-Methylisoxazol-3-amine hydrochloride → HCID 178428595, 화합물

HRID 1679368노트

반응식

HRID 1679368 반응식
[ClH:1].[NH2:2][C:3]1[CH:7]=[C:6]([CH3:8])[O:5][N:4]=1.[C:9]([NH:11][C:12]([NH2:14])=[NH:13])#[N:10]>C(O)CCC>[ClH:1].[CH3:8][C:6]1[O:5][N:4]=[C:3]([NH:2][C:9]([NH:11][C:12]([NH2:14])=[NH:13])=[NH:10])[CH:7]=1

참가 물질

4

반응물 2

HCID 203177225-Methylisoxazol-3-amine hydrochlorideHCID 178418324HCID 178418324, 화합물

생성물 1

HCID 178428595HCID 178428595, 화합물수율 41.6%

시약·촉매·용매 1

HCID 2631-Butanol용매

실험 절차

In a 2 liter three-necked flask are added 370 g of 3-amino-5-methyl-isoxazole hydrochloride, 231 g of 1-cyano-guanidine and 500 ml of butanol. The temperature is gradually raised to the refluxing temperature of the solvent, at which level it is then maintained during 10 minutes. The reaction mixture is allowed to cool and, after incipient crystallization, is poured over 2 liters of butanol. After complete crystallization, the resulting material is filtered, the solid is washed with 300 ml of isopropanol. The solid is recrystallized from 1 liter 90% ethanol, to give 250 g of (5-methyl-isoxazol-3-yl)biguanide hydrochloride. M.p. (Kofler) = 210°-212° C. M.p. (cap.) = 195°-196° C with introduction at 185° C and heating at a rate of 2° C/minute.

후처리

  1. temperatureThe temperature is gradually raised to the refluxing temperature of the solvent, at which level it
  2. temperatureis then maintained during 10 minutes
  3. temperatureto cool
  4. customafter incipient crystallization
  5. additionis poured over 2 liters of butanol
  6. customAfter complete crystallization
  7. filtrationthe resulting material is filtered
  8. washthe solid is washed with 300 ml of isopropanol
  9. customThe solid is recrystallized from 1 liter 90% ethanol

출처 및 근거

ORD 기록
ord-7ec9f9d6d7d74953a4f63238bf7a8a26
출처 데이터셋
uspto-grants-1978_03
특허 번호
US04080460

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