Ethanol → 5-Amino-3-isopropylisothiazole-4-carbonitrile

HRID 437698ノート

反応式

HRID 437698 の反応式
[NH2:1][C:2]([CH:9]([CH3:11])[CH3:10])=[C:3]([C:7]#[N:8])[C:4](=[S:6])[NH2:5].C(O)C.OO>O>[NH2:5][C:4]1[S:6][N:1]=[C:2]([CH:9]([CH3:11])[CH3:10])[C:3]=1[C:7]#[N:8]

参加物

5

反応物 3

HCID 702EthanolHCID 784Hydrogen PeroxideHCID 73793209HCID 73793209、化合物

生成物 1

HCID 152801535-Amino-3-isopropylisothiazole-4-carbonitrile収率 97.2%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

To a stirred mixture of 444.3 g of 3-amino-2-cyano-4-methyl-2-pentenethioamide (from part B) and 1315 ml of ethanol were added dropwise 298 g of 30% hydrogen peroxide (containing 89.4 g of active H2O2) during 1.25 hours. The reaction temperature was maintained at 30°-35° with an ice bath. The reaction mixture was stirred an additional 17.5-18 hours in an ambient temperature water bath. The reaction mixture was poured into 5100 ml of cold water with stirring. The water was cooled in an ice-water bath during addition of the reaction mixture. The mixture was stirred for one hour at 5°-10° and filtered. The filter cake was washed with 2 liters of water and allowed to dry on the suction filter. After air-drying over a weekend, 426.5 g of 5-amino-4-cyano-3-isopropylisothiazole, mp 130°-132° was obtained.

後処理

  1. temperatureThe reaction temperature was maintained at 30°-35° with an ice bath
  2. stirringwith stirring
  3. stirringThe mixture was stirred for one hour at 5°-10°
  4. filtrationfiltered
  5. washThe filter cake was washed with 2 liters of water
  6. customto dry on the suction
  7. filtrationfilter
  8. customAfter air-drying over a weekend

出典と根拠

ORDレコード
ord-6d6f07613d974b9199090137aec53b60
出典データセット
uspto-grants-1977_06
特許番号
US04032321

反応ノート

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