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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride → 2-(2-Benzothienyl)-3-oxa-1-azaspiro[4.5]dec-1-en-4-one

HRID 73855
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HRID 73855 반응식
Cl.C(N=C=NCCCN(C)C)C.[S:13]1[C:17]2[CH:18]=[CH:19][CH:20]=[CH:21][C:16]=2[CH:15]=[C:14]1[C:22]([NH:24][C:25]1([C:31]([OH:33])=[O:32])[CH2:30][CH2:29][CH2:28][CH2:27][CH2:26]1)=O>C(Cl)Cl>[S:13]1[C:17]2[CH:18]=[CH:19][CH:20]=[CH:21][C:16]=2[CH:15]=[C:14]1[C:22]1[O:33][C:31](=[O:32])[C:25]2([CH2:26][CH2:27][CH2:28][CH2:29][CH2:30]2)[N:24]=1
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참가 물질

4

반응물 2

HCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 432420401-[(2-Benzothienylcarbonyl)amino]cyclohexanecarboxylic acid

생성물 1

HCID 576728542-(2-Benzothienyl)-3-oxa-1-azaspiro[4.5]dec-1-en-4-one수율 76.7%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

4.1 g (21 mmol) of 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride was added to a solution of 5 g (16 mmol) of 1-[(2-benzothienylcarbonyl)amino]cyclohexanecarboxylic acid in 50 ml of methylene chloride. After the mixture was stirred at room temperature for 4 hours, the reaction solution was concentrated under reduced pressure, ethyl acetate was added thereto, and the mixture was successively washed with water, a 10% aqueous potassium hydrogensulfate solution, a saturated aqueous sodium hydrogencarbonate solution and saturated brine. The organic layer was dried with anhydrous sodium sulfate and the solvent was distilled off under reduced pressure to obtain 3.5 g (75%) of the title compound.

후처리

  1. concentrationthe reaction solution was concentrated under reduced pressure, ethyl acetate
  2. additionwas added
  3. washthe mixture was successively washed with water
  4. dry with materialThe organic layer was dried with anhydrous sodium sulfate
  5. distillationthe solvent was distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-48bf78085dae40148953adac9135e237
출처 데이터셋
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08829209B2

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