5-Methylisoxazol-3-amine hydrochloride → HCID 178428595、化合物

HRID 1679368ノート

反応式

HRID 1679368 の反応式
[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

参加物

4

反応物 2

HCID 203177225-Methylisoxazol-3-amine hydrochlorideHCID 178418324HCID 178418324、化合物

生成物 1

HCID 178428595HCID 178428595、化合物収率 41.6%

試薬・触媒・溶媒 1

HCID 2631-Butanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-7ec9f9d6d7d74953a4f63238bf7a8a26
出典データセット
uspto-grants-1978_03
特許番号
US04080460

反応ノート

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