Morpholine → Morpholine, 4-(2,4-dinitrophenylbenzoyl)-

HRID 1087170

反応式

HRID 1087170 の反応式
[N+:1]([C:4]1[CH:12]=[C:11]([N+:13]([O-:15])=[O:14])[CH:10]=[CH:9][C:5]=1[C:6]([OH:8])=O)([O-:3])=[O:2].[NH:16]1[CH2:21][CH2:20][O:19][CH2:18][CH2:17]1.P(Cl)(Cl)(Cl)=O.C([O-])(O)=O.[Na+]>C1(C)C=CC=CC=1>[N+:1]([C:4]1[CH:12]=[C:11]([N+:13]([O-:15])=[O:14])[CH:10]=[CH:9][C:5]=1[C:6]([N:16]1[CH2:21][CH2:20][O:19][CH2:18][CH2:17]1)=[O:8])([O-:3])=[O:2]

参加物

6

反応物 4

HCID 8083MorpholineHCID 118802,4-Dinitrobenzoic acidHCID 24813Phosphorus oxychlorideHCID 516892Sodium Bicarbonate

生成物 1

HCID 544864Morpholine, 4-(2,4-dinitrophenylbenzoyl)-収率 81.2%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
80 °C

実験手順

To a slurry of 215.1 g of 2,4-dinitrobenzoic acid in 1000 ml of toluene was added with stirring 196.2 g of morpholine. Next 76.5 g of phosphorus oxychloride was added dropwise at such a rate to maintain the reaction temperature below 90° C. The mixture was refluxed for 5 hrs, cooled to 80° C., and slowly poured into 1000 ml of aqueous 5% NaHCO3 solution with stirring. The precipitate was filtered, washed with water and dried to yield 231.7 g of N-(2,4-dinitrobenzoyl)morpholine, mp 159°-161° C.

後処理

  1. temperatureto maintain the reaction temperature below 90° C
  2. temperatureThe mixture was refluxed for 5 hrs
  3. filtrationThe precipitate was filtered
  4. washwashed with water
  5. customdried

出典と根拠

ORDレコード
ord-f3a7b5a8a6944e42a08d0ec5072c6f9e
出典データセット
uspto-grants-1991_07
特許番号
US05034426

関連ノート

読み込み中…