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Water → N-(5-ethyl-1,3,4-oxadiazol-2-yl)-4-(3-phenyl-1,2,4-thiadiazol-5-yl)piperazine-1-carboxamide

HRID 2262952
ノート
印刷プレビュー

反応式

HRID 2262952 の反応式
[CH2:1]([C:3]1[O:7][C:6]([NH:8][C:9](=[O:16])OCC(Cl)(Cl)Cl)=[N:5][N:4]=1)[CH3:2].[C:17]1([C:23]2[N:27]=[C:26]([N:28]3[CH2:33][CH2:32][NH:31][CH2:30][CH2:29]3)[S:25][N:24]=2)[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1.C(N(C(C)C)CC)(C)C.O>CS(C)=O>[CH2:1]([C:3]1[O:7][C:6]([NH:8][C:9]([N:31]2[CH2:32][CH2:33][N:28]([C:26]3[S:25][N:24]=[C:23]([C:17]4[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=4)[N:27]=3)[CH2:29][CH2:30]2)=[O:16])=[N:5][N:4]=1)[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 81531DiisopropylethylamineHCID 27777601-(3-Phenyl-(1,2,4)thiadiazol-5-yl)-piperazineHCID 862451962,2,2-Trichloroethyl (5-ethyl-1,3,4-oxadiazol-2-yl)carbamate

生成物 1

HCID 68777817N-(5-ethyl-1,3,4-oxadiazol-2-yl)-4-(3-phenyl-1,2,4-thiadiazol-5-yl)piperazine-1-carboxamide

試薬・触媒・溶媒 1

HCID 679
Dimethyl Sulfoxide
溶媒

実験手順

A mixed solution of 2,2,2-trichloroethyl (5-ethyl-1,3,4-oxadiazol-2-yl)carbamate (213 mg, 0.738 mmol), 1-(3-phenyl-1,2,4-thiadiazol-5-yl)piperazine (200 mg, 0.812 mmol) and diisopropylethylamine (0.129 ml, 0.738 mmol) in dimethyl sulfoxide (2.5 ml) was stirred at 70° C. for 3 hours and half. Water was poured to the reaction mixture, and the resulting solution was extracted with ethyl acetate. The extract was washed with water and dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. Chloroform was poured to the residue, and 140 mg (49.1%) of the desired product as a solid was separated by filtration.

後処理

  1. extractionthe resulting solution was extracted with ethyl acetate
  2. washThe extract was washed with water
  3. dry with materialdried over anhydrous magnesium sulfate
  4. distillationthe solvent was distilled off under reduced pressure
  5. additionChloroform was poured to the residue, and 140 mg (49.1%) of the desired product as a solid
  6. customwas separated by filtration

出典と根拠

ORDレコード
ord-31d8a92e0f9845988ec2b84ac1510c4f
出典データセット
uspto-grants-2010_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07851473B2

反応ノート

読み込み中…

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