Ammonium cerium (IV) nitrate → HCID 53699063、化合物

HRID 372325ノート

反応式

HRID 372325 の反応式
[N+]([O-])([O-])=O.[NH4+].[Ce+4].[N+]([O-])([O-])=O.[N+]([O-])([O-])=O.[N+]([O-])([O-])=O.[N+]([O-])([O-])=[O:20].[CH2:23]([O:25][C:26]([C:28]1[O:29][C:30]([C:37]2[CH:42]=[CH:41][C:40]([Cl:43])=[CH:39][CH:38]=2)=[C:31]2[C:36]=1[CH:35]=[CH:34][CH:33]=[CH:32]2)=[O:27])[CH3:24]>O>[CH2:23]([O:25][C:26](=[O:27])[C:28]([C:36]1[CH:35]=[CH:34][CH:33]=[CH:32][C:31]=1[C:30](=[O:29])[C:37]1[CH:42]=[CH:41][C:40]([Cl:43])=[CH:39][CH:38]=1)=[O:20])[CH3:24]

参加物

4

反応物 2

HCID 9869224Ammonium cerium (IV) nitrateHCID 53839738Ethyl 3-(4-chlorophenyl)-2-benzofuran-1-carboxylate

生成物 1

HCID 53699063HCID 53699063、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

11.5 G. of cerium (IV) ammonium nitrate are dissolved in 20 ml. of water and 20 ml. of glacial acid. Thereafter, there are added 3.0 g. of 3-(p-chlorophenyl)-isobenzofuran-1-carboxylic acid ethyl ester and the mixture is boiled for 2-3 minutes until the color of the solution obtained changes from orange to light-yellow. After cooling, there are added 150 ml. of ice-water and the mixture is stirred for 1 hour in an ice-bath. The product which first separates as an oil solidifies. The solid is separated by decantation of the aqueous solution and is dissolved in ether. The ethereal solution is washed with 2-N sodium carbonate and water, dried over sodium sulfate and evaporated. After crystallization of the residue from ethanol, there is obtained [o-(p-chlorobenzoyl)-phenyl]glyoxylic acid ethyl ester in the form of colorless crystals having a melting point of 79°-81° C.

後処理

  1. additionThereafter, there are added 3.0 g
  2. customobtained changes from orange to light-yellow
  3. temperatureAfter cooling
  4. additionthere are added 150 ml
  5. customThe solid is separated by decantation of the aqueous solution
  6. dissolutionis dissolved in ether
  7. washThe ethereal solution is washed with 2-N sodium carbonate and water
  8. dry with materialdried over sodium sulfate
  9. customevaporated
  10. customAfter crystallization of the residue from ethanol

出典と根拠

ORDレコード
ord-cd8ab2cc8d314d7e9514176dc92ca9b1
出典データセット
uspto-grants-1978_05
特許番号
US04090027

反応ノート

読み込み中…