Hydrochloric Acid → 2-[1-(Ethoxyimino)propyl]-3-hydroxy-5-(4-methanesulfonamidophenyl)-2-cyclohexen-1-one

HRID 2164360노트

반응식

HRID 2164360 반응식
[OH:1][C:2]1[CH2:7][CH:6]([C:8]2[CH:13]=[CH:12][C:11]([NH:14][S:15]([CH3:18])(=[O:17])=[O:16])=[CH:10][CH:9]=2)[CH2:5][C:4](=[O:19])[C:3]=1[C:20](=O)[CH2:21][CH3:22].[CH2:24]([O:26][NH2:27])[CH3:25].Cl>O1CCCC1>[CH2:24]([O:26][N:27]=[C:20]([C:3]1[C:4](=[O:19])[CH2:5][CH:6]([C:8]2[CH:9]=[CH:10][C:11]([NH:14][S:15]([CH3:18])(=[O:17])=[O:16])=[CH:12][CH:13]=2)[CH2:7][C:2]=1[OH:1])[CH2:21][CH3:22])[CH3:25]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 69357Hydroxylamine, O-ethyl-HCID 178458872HCID 178458872, 화합물

생성물 1

HCID 1361023912-[1-(Ethoxyimino)propyl]-3-hydroxy-5-(4-methanesulfonamidophenyl)-2-cyclohexen-1-one수율 82.8%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Into 10 ml of tetrahydrofuran was dissolved 1.5 g of 3-hydroxy-5-(4-methanesulfonamidophenyl)-2-propionyl-2-cyclohexen-1-one and to the solution was added 0.5 g of ethoxyamine. The mixture was kept at room temperature for 15 hours and poured into ice water. And then the mixture was acidified with hydrochloric acid and it was extracted with chloroform. The chloroform solution was washed with water and extracted with 15 ml of an aqueous solution containing 5% of sodium hydroxide. The solution was acidified with hydrochloric acid and the crystal sedimented was extracted with chloroform and the solution was washed with water and it was dried with magnesium sulfate. Then, it was distilled off under a reduced pressure and thus, 1.4 g of the desired compound was obtained. It was in the form of colorless crystals having a melting point of 115°-116° C.

후처리

  1. extractionwas extracted with chloroform
  2. washThe chloroform solution was washed with water
  3. extractionextracted with 15 ml of an aqueous solution
  4. additioncontaining 5% of sodium hydroxide
  5. extractionthe crystal sedimented was extracted with chloroform
  6. washthe solution was washed with water and it
  7. dry with materialwas dried with magnesium sulfate
  8. distillationThen, it was distilled off under a reduced pressure

출처 및 근거

ORD 기록
ord-a9f60c5375924a04bab9f56f8405c2ee
출처 데이터셋
uspto-grants-1985_03
특허 번호
US04504305

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