Water → 1-(2,4-Dichlorophenyl)-3-hydroxyurea

HRID 1582552

반응식

HRID 1582552 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[N:9]=[C:10]=[O:11].Cl.[NH2:13][OH:14].[OH-].[Na+].O>C1(C)C=CC=CC=1>[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[NH:9][C:10]([NH:13][OH:14])=[O:11]

참가 물질

6

반응물 4

HCID 962WaterHCID 14798Sodium HydroxideHCID 757892,4-Dichlorophenyl isocyanateHCID 443297Hydroxyamine hydrochloride

생성물 1

HCID 42954891-(2,4-Dichlorophenyl)-3-hydroxyurea수율 76.6%

시약·촉매·용매 1

HCID 1140Toluene용매2회

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온도
25 °C

실험 절차

A solution of 14.2 g (75 mmol) of 2,4-dichlorophenylisocyanate in 50 mL of toluene was added to a mixture of 8.26 g (120 mmol) of hydroxylamine hydrochloride and 4.8 g (120 mmol) of sodium hydroxide in a two-phase solvent mixture consisting of 50 mL of water and 50 mL of toluene. The resulting mixture was stirred at 25° C. for 30 minutes and filtered. The solid thus obtained was washed with water and then dissolved in 200 mL of ethyl acetate. The solution was dried over magnesium sulfate and the solvent was removed under reduced pressure to yield 12.7 g of the title compound of Step A as a white solid melting at 157-158° C. It was used directly in the next step without further purification.

후처리

  1. filtrationfiltered
  2. customThe solid thus obtained
  3. washwas washed with water
  4. dissolutiondissolved in 200 mL of ethyl acetate
  5. dry with materialThe solution was dried over magnesium sulfate
  6. customthe solvent was removed under reduced pressure

출처 및 근거

ORD 기록
ord-cd4a5e9706a14379bd3486860ef85942
출처 데이터셋
uspto-grants-2004_05
특허 번호
US06737383B1

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