N-bromobutanimide → HCID 22282008、化合物

HRID 1062817ノート

反応式

HRID 1062817 の反応式
[Br:1]N1C(=O)CCC1=O.[CH3:9][O:10][C:11]1[CH:23]=[CH:22][CH:21]=[CH:20][C:12]=1[O:13][CH2:14][C:15]([O:17][CH2:18][CH3:19])=[O:16]>C(Cl)(Cl)(Cl)Cl>[Br:1][CH:14]([O:13][C:12]1[CH:20]=[CH:21][CH:22]=[CH:23][C:11]=1[O:10][CH3:9])[C:15]([O:17][CH2:18][CH3:19])=[O:16]

参加物

4

反応物 2

HCID 67184N-bromobutanimideHCID 83114Ethyl (2-methoxyphenoxy)acetate

生成物 1

HCID 22282008HCID 22282008、化合物収率 105.9%

試薬・触媒・溶媒 1

HCID 5943Carbon Tetrachloride溶媒

実験手順

A solution of N-bromosuccinimide (13.35 g), azoisobutyronitrile (200 mg) and ethyl 2-(2-methoxyphenoxy)acetate (15.1 g) in anhydrous carbon tetrachloride (ex. calcium hydride) (100 ml) was irradiated with a 120 W sunlamp under reflux and a nitrogen atmosphere for 7 hours. The resulting suspension was allowed to stand at room temperature for 72 hours and was then filtered to remove the suspended solids, which were washed with toluene (40 ml). The combined filtrates were evaporated under vacuum leaving a brown liquid (22 g) Rf 0.75 (dichloromethane).

後処理

  1. temperatureunder reflux
  2. waitto stand at room temperature for 72 hours
  3. filtrationwas then filtered
  4. customto remove the suspended solids, which
  5. washwere washed with toluene (40 ml)
  6. customThe combined filtrates were evaporated under vacuum

出典と根拠

ORDレコード
ord-662eff709e7943da967ce5f65a344396
出典データセット
uspto-grants-2005_11
特許番号
US06962923B2

反応ノート

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