Water → phenylmethyl 1-[N-(4-methoxybenzenesulfonyl)amino]cyclohexanecarboxylate

HRID 1953445노트

반응식

HRID 1953445 반응식
[NH2:1][C:2]1([C:8]([O:10][CH2:11][C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)=[O:9])[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3]1.CC1C=CC(S(O)(=O)=O)=CC=1.O.[CH3:30][O:31][C:32]1[CH:37]=[CH:36][C:35]([S:38](Cl)(=[O:40])=[O:39])=[CH:34][CH:33]=1>C(OCC)(=O)C>[CH3:30][O:31][C:32]1[CH:33]=[CH:34][C:35]([S:38]([NH:1][C:2]2([C:8]([O:10][CH2:11][C:12]3[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=3)=[O:9])[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3]2)(=[O:40])=[O:39])=[CH:36][CH:37]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 74014-Methoxybenzenesulfonyl chlorideHCID 19763929Phenylmethyl 1-aminocyclohexanecarboxylate-p-toluenesulfonate

생성물 1

HCID 23297905phenylmethyl 1-[N-(4-methoxybenzenesulfonyl)amino]cyclohexanecarboxylate수율 54%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

8.1 g (20 mmol) of phenylmethyl 1-aminocyclohexanecarboxylate ·p-toluenesulfonate was added to 50 nm of water, and then 4.1 g (20 mmol) of 4-methoxybenzenesulfonylchloride and 50 ml of ethyl acetate was added to the mixture with stirring. After stirring at room temperature, the reaction mixture was put into a separatory funnel and water layer was removed therefrom. Subsequently, organic layer was washed with successive, 10% potassium hydrogensulfate solution, and saturated brine, and then, was dried over anhydrous magnesium sulfate, and the solvent was concentrated under reduced pressure. The obtained crystal was stirred overnight in ether, whereby 4.36 g of phenylmethyl 1-[N-(4-methoxybenzenesulfonyl)amino]cyclohexanecarboxylate was obtained.

후처리

  1. stirringAfter stirring at room temperature
  2. customthe reaction mixture was put into a separatory funnel
  3. customwater layer was removed
  4. washSubsequently, organic layer was washed with successive, 10% potassium hydrogensulfate solution, and saturated brine
  5. dry with materialwas dried over anhydrous magnesium sulfate
  6. concentrationthe solvent was concentrated under reduced pressure
  7. stirringThe obtained crystal was stirred overnight in ether

출처 및 근거

ORD 기록
ord-c32a8e12646547849f8b7d52975ba12c
출처 데이터셋
uspto-grants-2000_09
특허 번호
US06117870

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