Water → Phenyl 4-(methylcarbamoyl)phenylcarbamate

HRID 1871150노트

반응식

HRID 1871150 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

HCID 18321944Phenyl 4-(methylcarbamoyl)phenylcarbamate수율 94.5%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-2dc9156c1b5645b09d8526f4a3c39d0e
출처 데이터셋
uspto-grants-2000_08
특허 번호
US06100284

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