Water → Phenyl 4-(methylcarbamoyl)phenylcarbamate

HRID 1871150ノート

反応式

HRID 1871150 の反応式
[CH3:1][NH:2][C:3]([C:5]1[CH:11]=[CH:10][C:8]([NH2:9])=[CH:7][CH:6]=1)=[O:4].[OH-].[Na+].Cl[C:15]([O:17][C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)=[O:16].O>O1CCOCC1>[CH3:1][NH:2][C:3]([C:5]1[CH:11]=[CH:10][C:8]([NH:9][C:15](=[O:16])[O:17][C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)=[CH:7][CH:6]=1)=[O:4]

参加物

6

反応物 4

HCID 962WaterHCID 14798Sodium HydroxideHCID 15891Phenyl chloroformateHCID 2355164-Amino-N-methylbenzamide

生成物 1

HCID 18321944Phenyl 4-(methylcarbamoyl)phenylcarbamate収率 94.5%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

To a suspension of 4-(methylcarbamoyl)aniline (1.0 g) in 1,4-dioxane (10 ml) were added 1N sodium hydroxide solution (13.4 ml) and phenyl chloroformate (1.26 g) under ice-cooling, and the mixture was stirred for 2 hours at ambient temperature. The reaction mixture was poured into water and extracted with a mixture of chloroform and methanol. The extract was washed with water, dried over magnesium sulfate and evaporated in vacuo. The residue was crystallized from ethyl acetate to give phenyl 4-(methylcarbamoyl)phenylcarbamate (1.70 g) as pale yellow crystals.

後処理

  1. temperaturecooling
  2. extractionextracted with a mixture of chloroform and methanol
  3. washThe extract was washed with water
  4. dry with materialdried over magnesium sulfate
  5. customevaporated in vacuo
  6. customThe residue was crystallized from ethyl acetate

出典と根拠

ORDレコード
ord-2dc9156c1b5645b09d8526f4a3c39d0e
出典データセット
uspto-grants-2000_08
特許番号
US06100284

反応ノート

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