Water → Bis{5-Amino-1-(2,6-dichloro-4-trifluoromethylphenyl)-3-(1,2,4-oxadiazol-3-yl)pyrazol-4-yl}disulfide

HRID 429251노트

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HRID 429251 반응식
[NH2:1][C:2]1[N:6]([C:7]2[C:12]([Cl:13])=[CH:11][C:10]([C:14]([F:17])([F:16])[F:15])=[CH:9][C:8]=2[Cl:18])[N:5]=[C:4]([C:19]2[N:23]=[CH:22][O:21][N:20]=2)[C:3]=1[S:24]C#N.[BH4-].[Na+].[OH2:29]>CO>[NH2:1][C:2]1[N:6]([C:7]2[C:12]([Cl:13])=[CH:11][C:10]([C:14]([F:16])([F:17])[F:15])=[CH:9][C:8]=2[Cl:18])[N:5]=[C:4]([C:19]2[N:23]=[CH:22][O:29][N:20]=2)[C:3]=1[S:24][S:24][C:3]1[C:4]([C:19]2[N:23]=[CH:22][O:21][N:20]=2)=[N:5][N:6]([C:7]2[C:12]([Cl:13])=[CH:11][C:10]([C:14]([F:16])([F:15])[F:17])=[CH:9][C:8]=2[Cl:18])[C:2]=1[NH2:1]

참가 물질

5

반응물 3

HCID 962WaterHCID 4311764Sodium borohydrideHCID 155403545-Amino-1-(2,6-dichloro-4-trifluoromethylphenyl)-3-(1,2,4-oxadiazol-3-yl)-4-thiocyanato pyrazole

생성물 1

HCID 18354787Bis{5-Amino-1-(2,6-dichloro-4-trifluoromethylphenyl)-3-(1,2,4-oxadiazol-3-yl)pyrazol-4-yl}disulfide수율 55%

시약·촉매·용매 1

HCID 887Methanol용매

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온도
0 °C

실험 절차

5-Amino-1-(2,6-dichloro-4-trifluoromethylphenyl)-3-(1,2,4-oxadiazol-3-yl)-4-thiocyanatopyrazole 1.00 g (2.37 mmol) was dissolved in 20 ml of dry methanol, and then 210 mg (5.00 mmol) of 90% sodium borohydride was added at 0° C. After the mixture was was stirred at 0° C. for 3.5 hrs, the reaction mixture was poured into 80 ml iced water, and then the precipitate was collected by filtration. After drying in vacuo, the resulting yellow crystal was recrystalized from ethyl acetate-n-hexane mixed solvent to obtain 512 mg (0.65 mmol) of the title compound as a yellow crystal. Yield 55%.

후처리

  1. filtrationthe precipitate was collected by filtration
  2. customAfter drying in vacuo
  3. customthe resulting yellow crystal was recrystalized from ethyl acetate-n-hexane mixed solvent

출처 및 근거

ORD 기록
ord-2d6dc178cc0749db85c97e55976d0047
출처 데이터셋
uspto-grants-2001_11
특허 번호
US06316477B1

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