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

HRID 1953445ノート

反応式

HRID 1953445 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-c32a8e12646547849f8b7d52975ba12c
出典データセット
uspto-grants-2000_09
特許番号
US06117870

反応ノート

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