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Ethyl 3-(4-tert-butoxycarbonylaminocyclohex-1-enyl)benzoate → Ethyl 3-(4-aminocyclohex-1-enyl)benzoate

HRID 1425297
ノート
印刷プレビュー

反応式

HRID 1425297 の反応式
C(OC([NH:8][CH:9]1[CH2:14][CH2:13][C:12]([C:15]2[CH:16]=[C:17]([CH:23]=[CH:24][CH:25]=2)[C:18]([O:20][CH2:21][CH3:22])=[O:19])=[CH:11][CH2:10]1)=O)(C)(C)C>Cl.O1CCOCC1>[NH2:8][CH:9]1[CH2:14][CH2:13][C:12]([C:15]2[CH:16]=[C:17]([CH:23]=[CH:24][CH:25]=2)[C:18]([O:20][CH2:21][CH3:22])=[O:19])=[CH:11][CH2:10]1
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 1

HCID 67548489Ethyl 3-(4-tert-butoxycarbonylaminocyclohex-1-enyl)benzoate

生成物 1

HCID 67549303Ethyl 3-(4-aminocyclohex-1-enyl)benzoate収率 57.8%

試薬・触媒・溶媒 1

HCID 204431481,4-Dioxane hydrochloride溶媒

実験手順

A 4 N hydrochloric acid/1,4-dioxane solution (20 mL) was added to ethyl 3-(4-tert-butoxycarbonylaminocyclohex-1-enyl)benzoate obtained in Example (195b) (510 mg, 1.48 mmol). The mixture was stirred at room temperature for one hour, and the solvent was evaporated under reduced pressure. The resulting residue was dissolved in methanol. Amberlite IRA-400(Cl) ion exchange resin (20 g) was added, and the mixture was stirred at room temperature for one hour. Amberlite was filtered off, and then the solution was concentrated under reduced pressure to obtain 210 mg of the title compound as a colorless oily substance.

後処理

  1. customthe solvent was evaporated under reduced pressure
  2. dissolutionThe resulting residue was dissolved in methanol
  3. additionAmberlite IRA-400(Cl) ion exchange resin (20 g) was added
  4. stirringthe mixture was stirred at room temperature for one hour
  5. filtrationAmberlite was filtered off
  6. concentrationthe solution was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-88512e33c4374994955c8378833d9a9f
出典データセット
uspto-grants-2015_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08927588B2

反応ノート

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