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4-Methylmorpholine → [4-(2,4-Dimethylphenyl)-[1,4]diazepan-1-yl][4-(1,1-dioxo-1lambda6-isothiazolidin-2-yl)phenyl]methanone

HRID 2411477
ノート
印刷プレビュー

反応式

HRID 2411477 の反応式
[O:1]=[S:2]1(=[O:16])[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][CH:8]=1.Cl.[CH3:18][C:19]1[CH:24]=[C:23]([CH3:25])[CH:22]=[CH:21][C:20]=1[N:26]1[CH2:32][CH2:31][CH2:30][NH:29][CH2:28][CH2:27]1.CN1CCOCC1.O.[Cl-].COC1N=C(OC)N=C([N+]2(C)CCOCC2)N=1>CO.O1CCOCC1.O>[CH3:18][C:19]1[CH:24]=[C:23]([CH3:25])[CH:22]=[CH:21][C:20]=1[N:26]1[CH2:32][CH2:31][CH2:30][N:29]([C:11]([C:10]2[CH:9]=[CH:8][C:7]([N:3]3[CH2:4][CH2:5][CH2:6][S:2]3(=[O:1])=[O:16])=[CH:15][CH:14]=2)=[O:13])[CH2:28][CH2:27]1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 79724-MethylmorpholineHCID 66250114-(1,1-Dioxo-1,2-thiazolidin-2-yl)benzoic acidHCID 231494114-(4,6-Dimethoxy[1.3.5]triazin-2-yl)-4-methylmorpholinium chloride hydrateHCID 673808831-(2,4-Dimethylphenyl)-[1,4]diazepane hydrochloride

生成物 1

HCID 71252897[4-(2,4-Dimethylphenyl)-[1,4]diazepan-1-yl][4-(1,1-dioxo-1lambda6-isothiazolidin-2-yl)phenyl]methanone
収率 49.7%

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 962Water溶媒2 回HCID 312751,4-Dioxane溶媒

実験手順

A mixture of 4-(1,1-dioxo-1λ6-isothiazolidin-2-yl)benzoic acid (253 mg) described in Preparation Example 16, 1-(2,4-dimethylphenyl)-[1,4]diazepane hydrochloride (253 mg) described in Preparation Example 93 and N-methylmorpholine (0.12 mL) was dissolved in a solution of methanol (2 mL), 1,4-dioxane (2 mL) and water (0.5 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 overnight. 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 (223 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-32da236d9a4e49ac87a05a9c5fd562f3
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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