Dimethyl Sulfoxide → N-(3-Phenylisoxazol-5-yl)-4-(3-phenyl-1,2,4-thiadiazol-5-yl)piperazine-1-carboxamide

HRID 2263067

반응식

HRID 2263067 반응식
[C:1]1([C:7]2[CH:11]=[C:10]([NH:12][C:13](=[O:20])OCC(Cl)(Cl)Cl)[O:9][N:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[C:21]1([C:27]2[N:31]=[C:30]([N:32]3[CH2:37][CH2:36][NH:35][CH2:34][CH2:33]3)[S:29][N:28]=2)[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1.CS(C)=O>O>[C:1]1([C:7]2[CH:11]=[C:10]([NH:12][C:13]([N:35]3[CH2:36][CH2:37][N:32]([C:30]4[S:29][N:28]=[C:27]([C:21]5[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=5)[N:31]=4)[CH2:33][CH2:34]3)=[O:20])[O:9][N:8]=2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

참가 물질

5

반응물 3

HCID 679Dimethyl SulfoxideHCID 27777601-(3-Phenyl-(1,2,4)thiadiazol-5-yl)-piperazineHCID 862452722,2,2-Trichloroethyl (3-phenylisoxazol-5-yl)carbamate

생성물 1

HCID 68779635N-(3-Phenylisoxazol-5-yl)-4-(3-phenyl-1,2,4-thiadiazol-5-yl)piperazine-1-carboxamide수율 71.8%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A solution of 2,2,2-trichloroethyl (3-phenylisoxazol-5-yl)carbamate (336 mg, 1.00 mmol), 1-(3-phenyl-1,2,4-thiadiazol-5-yl)piperazine (246 mg, 1.00 mmol) diisopropylethylamine (0.174 ml, 1.00 mmol) and dimethylsulfoxide (5 ml) was stirred at 70° C. for 12 hours, the reaction mixture was poured into water and a solid was collected by filtration. This was recrystallized from a mixed solvent of tetrahydrofuran and ethyl acetate to obtain the desired product (310 mg, 71.8%) as a solid.

후처리

  1. filtrationa solid was collected by filtration
  2. customThis was recrystallized from a mixed solvent of tetrahydrofuran and ethyl acetate

출처 및 근거

ORD 기록
ord-5826262ce3084f7b9ad6521f1c1b843e
출처 데이터셋
uspto-grants-2010_12
특허 번호
US07851473B2

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