Water → HCID 12901252, 화합물

HRID 1589207노트

반응식

HRID 1589207 반응식
[NH2:1][C:2]1[C:7]([C:8](=[O:16])[C:9]2[CH:14]=[CH:13][C:12]([Cl:15])=[CH:11][CH:10]=2)=[CH:6][CH:5]=[CH:4][C:3]=1[CH2:17][C:18]([OH:20])=[O:19].[Na].O.[CH2:23](I)[CH3:24]>CN(C)C=O>[NH2:1][C:2]1[C:7]([C:8](=[O:16])[C:9]2[CH:14]=[CH:13][C:12]([Cl:15])=[CH:11][CH:10]=2)=[CH:6][CH:5]=[CH:4][C:3]=1[CH2:17][C:18]([O:20][CH2:23][CH3:24])=[O:19]

참가 물질

6

반응물 4

HCID 962Water2회HCID 6340IodoethaneHCID 173842Ahr 6293HCID 5360545Sodium

생성물 1

HCID 12901252HCID 12901252, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

Fourteen g of 2-amino-3-(4-chlorobenzoyl)benzene acetic acid, sodium salt.H2O was dissolved in 150 ml of dimethylformamide and then treated with 30 g of ethyl iodide. The resulting solution was stirred at room temperature for 2.5 hours. The solution was then added to water and the mixture was extracted several times with benzene. The benzene layer obtained was washed with dilute base and water, dried over sodium sulfate and stripped to leave an oil which crystallized on trituration with pet. ether. Recrystallization from ethyl alcohol gave 11.6 g of the titled compound as yellow flakes, m.p. 101°-102° C.

후처리

  1. extractionthe mixture was extracted several times with benzene
  2. customThe benzene layer obtained
  3. washwas washed
  4. additionwith dilute base and water
  5. dry with materialdried over sodium sulfate
  6. customto leave an oil which
  7. customcrystallized on trituration with pet. ether
  8. customRecrystallization from ethyl alcohol

출처 및 근거

ORD 기록
ord-87062308bf374ce2830aa886862b8b8b
출처 데이터셋
uspto-grants-1986_02
특허 번호
US04568695

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