Triethylamine → (4-Cyano-5-methyl-4-(3-cyano-2-thienyl)hexyl]-4-[2-(3-cyanophenoxy)ethyl]piperazine

HRID 1071650ノート

反応式

HRID 1071650 の反応式
[C:1]([C:3]([C:11]1[S:12][CH:13]=[CH:14][C:15]=1[C:16]#[N:17])([CH:8]([CH3:10])[CH3:9])[CH2:4][CH2:5][CH2:6]I)#[N:2].C(N(CC)CC)C.[C:25]([C:27]1[CH:28]=[C:29]([CH:39]=[CH:40][CH:41]=1)[O:30][CH2:31][CH2:32][N:33]1[CH2:38][CH2:37][NH:36][CH2:35][CH2:34]1)#[N:26]>C(#N)C>[C:1]([C:3]([C:11]1[S:12][CH:13]=[CH:14][C:15]=1[C:16]#[N:17])([CH:8]([CH3:10])[CH3:9])[CH2:4][CH2:5][CH2:6][N:36]1[CH2:35][CH2:34][N:33]([CH2:32][CH2:31][O:30][C:29]2[CH:39]=[CH:40][CH:41]=[C:27]([C:25]#[N:26])[CH:28]=2)[CH2:38][CH2:37]1)#[N:2]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 223936831-(3-Cyanophenoxyethyl)piperazineHCID 223938264-Cyano-5-methyl-4-(3-cyano-2-thienyl)hexyl iodide

生成物 1

HCID 22393576(4-Cyano-5-methyl-4-(3-cyano-2-thienyl)hexyl]-4-[2-(3-cyanophenoxy)ethyl]piperazine

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

In 1.5 ml of acetonitrile was dissolved 111 mg (0.31 mmol) of 4-cyano-5-methyl-4-(3-cyano-2-thienyl)hexyl iodide. To the mixture were added 56.2 μl (0.40 mmol) of triethylamine and 109 mg (0.47 mmol) of 1-(3-cyanophenoxyethyl)piperazine, followed by stirring for 3 days. The organic layer separated by adding ethyl acetate and brine to the reaction solution was dried over magnesium sulfate, and then evaporated, to give a crude product. The crude product was subjected to 12.5 g of Cromatorex NH silica gel (ethyl acetate/hexane-1/2), to give 144 mg (quantitative) of the title compound as a yellow syrup.

後処理

  1. customThe organic layer separated
  2. additionby adding ethyl acetate and brine to the reaction solution
  3. dry with materialwas dried over magnesium sulfate
  4. customevaporated
  5. customto give a crude product

出典と根拠

ORDレコード
ord-8c2c141c6ce34d538687ccdb5f8b6e93
出典データセット
uspto-grants-2005_06
特許番号
US06906072B1

反応ノート

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