Dimethylformamide → HCID 54385684、化合物

HRID 2231959ノート

反応式

HRID 2231959 の反応式
O=P(Cl)(Cl)Cl.[NH2:6][C:7]1[S:11][N:10]=[C:9]([C:12]([NH2:14])=O)[C:8]=1[C:15]([NH2:17])=O.[CH3:18][N:19]([CH3:22])[CH:20]=O>>[CH3:18][N:19]([CH3:22])[CH:20]=[N:6][C:7]1[S:11][N:10]=[C:9]([C:12]#[N:14])[C:8]=1[C:15]#[N:17]

参加物

4

反応物 3

HCID 6228DimethylformamideHCID 24813Phosphorus oxychlorideHCID 21285250HCID 21285250、化合物

生成物 1

HCID 54385684HCID 54385684、化合物収率 93%

実験手順

10.1 parts of phosphorus oxytrichloride are added dropwise to 30 parts of dimethylformamide at 0° C., and the mixture is then stirred for a further 0.5 hour at this temperature. 3.7 parts of 5-aminoisothiazole-3,4-dicarboxamide are then introduced, a little at a time, into this solution while cooling with ice. The mixture is stirred for a further 2 hours at room temperature, after which it is poured into 100 parts of ice water. The precipitate is filtered off under suction, washed with water and dried to give 3.8 parts (93% of theory) of N,N-dimethyl-N'-(3,4-dicyanoisothiazol-5-yl)-formamidine.

後処理

  1. temperaturea little at a time, into this solution while cooling with ice
  2. stirringThe mixture is stirred for a further 2 hours at room temperature
  3. filtrationThe precipitate is filtered off under suction
  4. washwashed with water
  5. customdried

出典と根拠

ORDレコード
ord-d95fc5374a504742a1142f2c6328272c
出典データセット
uspto-grants-1988_11
特許番号
US04785116

反応ノート

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