Nickel(II) bromide ethylene glycol dimethyl ether complex → HCID 86651358、化合物

HRID 416205ノート

反応式

HRID 416205 の反応式
[Ni:1]([Br:3])[Br:2].COCCOC.[CH3:10][Si:11]([CH3:29])([CH3:28])[C:12]1[CH:13]=[CH:14][C:15]([C:18]2[CH:23]=[CH:22][C:21]([Si:24]([CH3:27])([CH3:26])[CH3:25])=[CH:20][N:19]=2)=[N:16][CH:17]=1>C(O)C>[Ni:1]([Br:3])[Br:2].[CH3:25][Si:24]([CH3:27])([CH3:26])[C:21]1[CH:22]=[CH:23][C:18]([C:15]2[CH:14]=[CH:13][C:12]([Si:11]([CH3:29])([CH3:28])[CH3:10])=[CH:17][N:16]=2)=[N:19][CH:20]=1

参加物

4

反応物 2

HCID 6098672Nickel(II) bromide ethylene glycol dimethyl ether complexHCID 12984525HCID 12984525、化合物

生成物 1

HCID 86651358HCID 86651358、化合物収率 42.3%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a glass reaction container equipped with a cooling apparatus, 2.5 g of nickel bromide•ethylene glycol dimethyl ether, 2.56 g of 5,5′-bis(trimethylsilyl)-2,2′-bipyridine and 14 mL of ethanol were added at room temperature under a nitrogen atmosphere. The obtained mixture was reacted at 65° C. for 2 hours to obtain a crude product. The obtained crude product was recrystallized using hexane and ethanol to obtain 1.78 g of 5,5′-bis(trimethylsilyl)-2,2′-bipyridine nickel dibromide.

後処理

  1. customTo a glass reaction container
  2. additionwere added at room temperature under a nitrogen atmosphere
  3. customThe obtained mixture was reacted at 65° C. for 2 hours
  4. customto obtain a crude product
  5. customThe obtained crude product
  6. customwas recrystallized

出典と根拠

ORDレコード
ord-4b084f58c9a94dfd91cf4c2311e17d6f
出典データセット
uspto-grants-2012_01
特許番号
US08088883B2

反応ノート

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