Dimethylformamide → HCID 54385684, 화합물

HRID 2231959노트

반응식

HRID 2231959 반응식
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]

참가 물질

4

반응물 3

HCID 6228DimethylformamideHCID 24813Phosphorus oxychlorideHCID 21285250HCID 21285250, 화합물

생성물 1

HCID 54385684HCID 54385684, 화합물수율 93%

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d95fc5374a504742a1142f2c6328272c
출처 데이터셋
uspto-grants-1988_11
특허 번호
US04785116

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