2,4,5-Tribromoimidazole → 1-(4-Bromobutoxymethyl)-2,4,5-tribromoimidazole

HRID 1789342ノート

反応式

HRID 1789342 の反応式
[Na].[Br:2][C:3]1[NH:4][C:5]([Br:9])=[C:6]([Br:8])[N:7]=1.[H-].[Na+].[Br:12][CH2:13][CH2:14][CH2:15][CH2:16][O:17][CH2:18]Br>CN(C)C=O.O>[Br:12][CH2:13][CH2:14][CH2:15][CH2:16][O:17][CH2:18][N:4]1[C:5]([Br:9])=[C:6]([Br:8])[N:7]=[C:3]1[Br:2]

参加物

7

反応物 4

HCID 162532,4,5-TribromoimidazoleHCID 24758Sodium hydrideHCID 3146311-Bromo-4-(bromomethoxy)butaneHCID 5360545Sodium

生成物 1

HCID 139222111-(4-Bromobutoxymethyl)-2,4,5-tribromoimidazole収率 39.3%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

To a solution of a sodium salt, prepared from 1.22 g of 2,4,5-tribromoimidazole and 0.16 g of 60% oil-based sodium hydride, in 5 ml of N,N-dimethylformamide was added dropwise 1.23 g of 4-bromobutoxymethyl bromide at room temperature. After stirring at room temperature for 3 hours, 50 ml of water was added to the reaction mixture which was then extracted with three 30-ml portions of ether. The ether layer was dried over magnesium sulfate and concentrated. The oily product obtained was purified by column chromatography on silica gel to obtain 0.74 g of 1-(4-bromobutoxymethyl)-2,4,5-tribromoimidazole.

後処理

  1. extractionwas then extracted with three 30-ml portions of ether
  2. dry with materialThe ether layer was dried over magnesium sulfate
  3. concentrationconcentrated
  4. customThe oily product obtained
  5. customwas purified by column chromatography on silica gel

出典と根拠

ORDレコード
ord-d34625343e7649b5af49a1270004d653
出典データセット
uspto-grants-1987_08
特許番号
US04689340

反応ノート

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