Potassium Iodide → HCID 70290042、化合物

HRID 369767

反応式

HRID 369767 の反応式
[NH2:1][CH2:2][CH2:3][N:4]1[CH2:9][CH2:8][N:7]([C:10]2[C:19]3[O:18][CH2:17][CH2:16][O:15][C:14]=3[CH:13]=[CH:12][CH:11]=2)[CH2:6][CH2:5]1.BrC[CH:22]=[O:23].[I-].[K+].C(=O)([O-])[O-].[K+].[K+].O1[CH2:37][CH2:36][O:35][CH2:34]C1>C(OCC)(=O)C.CO.O>[O:15]1[C:14]2[CH:13]=[CH:12][CH:11]=[C:10]([N:7]3[CH2:6][CH2:5][N:4]([CH2:3][CH2:2][NH:1][CH2:37][CH:36]([O:35][CH3:34])[O:23][CH3:22])[CH2:9][CH2:8]3)[C:19]=2[O:18][CH2:17][CH2:16]1

参加物

8

反応物 5

HCID 4875Potassium IodideHCID 11430Potassium CarbonateHCID 312751,4-DioxaneHCID 105131Acetaldehyde, bromo-HCID 105876411-(2-Amino-1-ethyl)-4-(1,4-benzodioxan-5-yl)piperazine

生成物 1

HCID 70290042HCID 70290042、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 21584119Ethylacetate methanol溶媒

実験手順

A mixture of 1-(2-amino-1-ethyl)-4-(1,4-benzodioxan-5-yl)piperazine (9.1 g), bromoacetaldehyde dimethylacetale (6.5 g), potassium iodide (0.5 g), and potassium carbonate (4.8 g) in 1,4-dioxan (200 ml) was refluxed for 16 h. Water was added followed by extraction with ethyl acetate. The organic phase was concentrated in vacuo leaving an oil which was applied to a silica gel column (eluent: ethyl acetate/methanol=1:3). The product, 1-(1,4-benzodioxan-5-yl)-4-[2-(2,2-dimethoxy-1-ethylamino)-1-ethyl]piperazine, was obtained as an oil (4.7 g).

後処理

  1. temperaturewas refluxed for 16 h
  2. extractionfollowed by extraction with ethyl acetate
  3. concentrationThe organic phase was concentrated in vacuo
  4. customleaving an oil which

出典と根拠

ORDレコード
ord-a9408372408f465faf1f6e2346ffb2fa
出典データセット
uspto-grants-2000_10
特許番号
US06140331

関連ノート

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