Water → N-1,2-Benzisoxazol-3-yl-4-[3-(4-chlorophenyl)-1,2,4-thiadiazol-5-yl]piperazine-1-carboxamide

HRID 2262880ノート

反応式

HRID 2262880 の反応式
Cl[C:2]1[S:6][N:5]=[C:4]([C:7]2[CH:12]=[CH:11][C:10]([Cl:13])=[CH:9][CH:8]=2)[N:3]=1.FC(F)(F)C(O)=O.[O:21]1[C:25]2[CH:26]=[CH:27][CH:28]=[CH:29][C:24]=2[C:23]([NH:30][C:31]([N:33]2[CH2:38][CH2:37][NH:36][CH2:35][CH2:34]2)=[O:32])=[N:22]1.C(N(CC)CC)C.O>CN(C)C=O>[O:21]1[C:25]2[CH:26]=[CH:27][CH:28]=[CH:29][C:24]=2[C:23]([NH:30][C:31]([N:33]2[CH2:38][CH2:37][N:36]([C:2]3[S:6][N:5]=[C:4]([C:7]4[CH:12]=[CH:11][C:10]([Cl:13])=[CH:9][CH:8]=4)[N:3]=3)[CH2:35][CH2:34]2)=[O:32])=[N:22]1

参加物

6

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 463184645-Chloro-3-(4-chlorophenyl)-1,2,4-thiadiazoleHCID 68778018N-1,2-Benzisoxazol-3-ylpiperazine-1-carboxamide trifluoroacetate

生成物 1

HCID 68780033N-1,2-Benzisoxazol-3-yl-4-[3-(4-chlorophenyl)-1,2,4-thiadiazol-5-yl]piperazine-1-carboxamide収率 34.7%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 5-chloro-3-(4-chlorophenyl)-1,2,4-thiadiazole (179 mg, 0.555 mmol) and N-1,2-benzisoxazol-3-ylpiperazine-1-carboxamide trifluoroacetate (200 mg, 0.555 mmol) in dimethylformamide (2 ml) was added triethylamine (0.389 ml, 2.78 mmol) at room temperature, and the mixture was stirred at room temperature for 2 hours. The reaction mixture was poured to water, and the precipitated solid was separated by filtration, which was recrystallized from a mixed solvent of ethyl acetate and tetrahydrofuran to give 85.0 mg (34.7%) of the desired product.

後処理

  1. customthe precipitated solid was separated by filtration, which
  2. customwas recrystallized from a mixed solvent of ethyl acetate and tetrahydrofuran

出典と根拠

ORDレコード
ord-77e4b5a0bc4d4ceb872092e1c8aae553
出典データセット
uspto-grants-2010_12
特許番号
US07851473B2

反応ノート

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