Sulfuric acid magnesium salt (1:1) → [4-(2-Pyrrolidin-1-yl-ethoxy)-phenyl]-[4-(tetrahydro-pyran-2-yloxy)-benzylidene]-amine

HRID 1827561

反応式

HRID 1827561 の反応式
[N:1]1([CH2:6][CH2:7][O:8][C:9]2[CH:14]=[CH:13][C:12]([NH2:15])=[CH:11][CH:10]=2)[CH2:5][CH2:4][CH2:3][CH2:2]1.[O:16]1[CH2:21][CH2:20][CH2:19][CH2:18][CH:17]1[O:22][C:23]1[CH:30]=[CH:29][C:26]([CH:27]=O)=[CH:25][CH:24]=1.S([O-])([O-])(=O)=O.[Mg+2]>C(Cl)Cl>[N:1]1([CH2:6][CH2:7][O:8][C:9]2[CH:10]=[CH:11][C:12]([N:15]=[CH:27][C:26]3[CH:25]=[CH:24][C:23]([O:22][CH:17]4[CH2:18][CH2:19][CH2:20][CH2:21][O:16]4)=[CH:30][CH:29]=3)=[CH:13][CH:14]=2)[CH2:5][CH2:4][CH2:3][CH2:2]1

参加物

5

反応物 3

HCID 24083Sulfuric acid magnesium salt (1:1)HCID 64937494-(2-(Pyrrolidin-1-yl)ethoxy)anilineHCID 112527364-(2-Tetrahydro-2H-pyranoxy)benzaldehyde

生成物 1

HCID 22137358[4-(2-Pyrrolidin-1-yl-ethoxy)-phenyl]-[4-(tetrahydro-pyran-2-yloxy)-benzylidene]-amine収率 100.6%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 4-(2-pyrrolidin-1-yl-ethoxy)-phenylamine (6.92 g, 33.5 mmol) and 4-(tetrahydro-pyran-2-yloxy)-benzaldehyde (7.25 g, 35.2 mmol) in 110 mL methylene chloride was added magnesium sulfate (14.2 g, 117.3 mmol). The reaction mixture was stirred at room temperature overnight under nitrogen. The reaction was filtered and concentrated to afford 13.3 g of the crude title compound of Step A which was used without further purification. MS 395.2 (M+1)+

後処理

  1. filtrationThe reaction was filtered
  2. concentrationconcentrated

出典と根拠

ORDレコード
ord-4e8070cd2fab4b04af5c745f8716d90e
出典データセット
uspto-grants-2006_05
特許番号
US07053212B2

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