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

HRID 1789342노트

반응식

HRID 1789342 반응식
[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]

참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d34625343e7649b5af49a1270004d653
출처 데이터셋
uspto-grants-1987_08
특허 번호
US04689340

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