Hydrochloric Acid → HCID 53858733, 화합물

HRID 1494003

반응식

HRID 1494003 반응식
[CH3:1][O:2][C:3]1[CH:4]=[CH:5][CH:6]=[CH:7][C:8]=1[O:9][CH2:10][CH:11](O)[CH2:12][OH:13].N1C=CC=CC=1.[CH2:21]([NH:23][S:24](Cl)(=[O:26])=[O:25])[CH3:22].Cl>C(Cl)Cl>[CH3:1][O:2][C:3]1[CH:4]=[CH:5][CH:6]=[CH:7][C:8]=1[O:9][CH2:10][CH2:11][CH2:12][O:13][S:24](=[O:26])(=[O:25])[NH:23][CH2:21][CH3:22]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 1049PyridineHCID 3516GuaifenesinHCID 11040810Ethylsulfamoyl chloride

생성물 1

HCID 53858733HCID 53858733, 화합물수율 69.8%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

A solution of 19.8 g (0.1 mole) of glyceryl guaiacolate in 100 ml of methylene chloride and 21.6 ml (0.26 mole) of pyridine was added in a thin stream to a stirred solution of 37.3 g (0.26 mole) of ethysulfamoyl chloride (prepared using procedure of Example 2, pt. a) in 150 ml of methylene chloride, and the reaction mixture was stirred at ambient temperature overnight. The reaction mixture was treated with 150 ml of 2N hydrochloric acid solution, and the layers were separated. The organic layer was washed with 150 ml of 2N hydrochloric acid solution, twice with 150 ml portions of water, dried (magnesium sulfate), and the solvent was evaporated under reduced pressure. The residue was purified by chromatography (4.5×90 cm glass column; 500 g of silica gel; methylene chloride-acetone, 25:1). Fractions containing the product were combined, and the solvents wre evaporated under reduced pressure to give 20.2 g (49%) of the title compound as a light-yellow, viscous oil containing a trace of methylene chloride.

후처리

  1. customprepared
  2. customthe layers were separated
  3. washThe organic layer was washed with 150 ml of 2N hydrochloric acid solution, twice with 150 ml portions of water
  4. dry with materialdried (magnesium sulfate)
  5. customthe solvent was evaporated under reduced pressure
  6. customThe residue was purified by chromatography (4.5×90 cm glass column; 500 g of silica gel; methylene chloride-acetone, 25:1)
  7. additionFractions containing the product
  8. customthe solvents wre evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-2a8af2add32d439e80b766bb945ed395
출처 데이터셋
uspto-grants-1991_06
특허 번호
US05025031

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