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Water → [4-(2,4-Dimethylphenyl)piperazin-1-yl][4-(1,1-dioxo-1lambda6-isothiazolidin-2-yl)-3-methoxyphenyl]methanone

HRID 2411473
ノート
印刷プレビュー

反応式

HRID 2411473 の反応式
[O:1]=[S:2]1(=[O:18])[CH2:6][CH2:5][CH2:4][N:3]1[C:7]1[CH:15]=[CH:14][C:10]([C:11]([OH:13])=O)=[CH:9][C:8]=1[O:16][CH3:17].[CH3:19][C:20]1[CH:25]=[C:24]([CH3:26])[CH:23]=[CH:22][C:21]=1[N:27]1[CH2:32][CH2:31][NH:30][CH2:29][CH2:28]1.O.[Cl-].COC1N=C(OC)N=C([N+]2(C)CCOCC2)N=1.O>C(Cl)(Cl)Cl.CO>[CH3:19][C:20]1[CH:25]=[C:24]([CH3:26])[CH:23]=[CH:22][C:21]=1[N:27]1[CH2:28][CH2:29][N:30]([C:11]([C:10]2[CH:14]=[CH:15][C:7]([N:3]3[CH2:4][CH2:5][CH2:6][S:2]3(=[O:1])=[O:18])=[C:8]([O:16][CH3:17])[CH:9]=2)=[O:13])[CH2:31][CH2:32]1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 962WaterHCID 705441-(2,4-Xylyl)piperazineHCID 231494114-(4,6-Dimethoxy[1.3.5]triazin-2-yl)-4-methylmorpholinium chloride hydrateHCID 712525024-(1,1-Dioxo-1lambda6-isothiazolidin-2-yl)-3-methoxybenzoic acid

生成物 1

HCID 71252668[4-(2,4-Dimethylphenyl)piperazin-1-yl][4-(1,1-dioxo-1lambda6-isothiazolidin-2-yl)-3-methoxyphenyl]methanone収率 88.6%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 6212Chloroform溶媒

実験手順

4-(1,1-Dioxo-1λ6-isothiazolidin-2-yl)-3-methoxybenzoic acid (285 mg) described in Preparation Example 21 and 1-(2,4-dimethylphenyl)piperazine (199 mg) were dissolved in a solution of chloroform (2.1 mL) and methanol (2.1 mL), 4-(4,6-dimethoxy[1.3.5]triazin-2-yl)-4-methylmorpholinium chloride hydrate (349 mg) was added, and the mixture was stirred at room temperature. Water was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, and the solvent was evaporated. The obtained residue was purified by column chromatography (chloroform:methanol) to give the title compound (411 mg).

後処理

  1. additionwas added
  2. extractionthe mixture was extracted with ethyl acetate
  3. washThe organic layer was washed with saturated brine
  4. customthe solvent was evaporated
  5. customThe obtained residue was purified by column chromatography (chloroform:methanol)

出典と根拠

ORDレコード
ord-07ccbff127e741c6b77df4bf7ee76613
出典データセット
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08816079B2

反応ノート

読み込み中…

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