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Diethyl Ether → 1-[(2-Benzothienylcarbonyl)amino]cyclohexanecarboxylic acid

HRID 1627475
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HRID 1627475 반응식
[OH-].[Na+].C1(C[O:10][C:11]([C:13]2([NH:19][C:20]([C:22]3[S:23][C:24]4[CH:30]=[CH:29][CH:28]=[CH:27][C:25]=4[CH:26]=3)=[O:21])[CH2:18][CH2:17][CH2:16][CH2:15][CH2:14]2)=[O:12])C=CC=CC=1.CCOCC>O1CCCC1>[S:23]1[C:24]2[CH:30]=[CH:29][CH:28]=[CH:27][C:25]=2[CH:26]=[C:22]1[C:20]([NH:19][C:13]1([C:11]([OH:12])=[O:10])[CH2:18][CH2:17][CH2:16][CH2:15][CH2:14]1)=[O:21]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 3283Diethyl EtherHCID 14798Sodium HydroxideHCID 576728971-[(2-Benzothienylcarbonyl)amino]cyclohexanecarboxylic acid phenylmethyl ester

생성물 1

HCID 432420401-[(2-Benzothienylcarbonyl)amino]cyclohexanecarboxylic acid수율 83.8%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

42 ml of 2N aqueous sodium hydroxide solution was added to a solution of 10 g (24 mmol) of 1-[(2-benzothienylcarbonyl)amino]cyclohexanecarboxylic acid phenylmethyl ester in 20 ml of tetrahydrofuran, and the mixture was heated under reflux for 3 days. After ether was added to the reaction solution to wash it, the aqueous layer was neutralized by concentrated hydrochloric acid and the precipitated crystal was collected by filtration. The obtained crystal was dried under reduced pressure to obtain 6.1 g (80%) of the title compound.

후처리

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 3 days
  3. washto wash it
  4. filtrationthe precipitated crystal was collected by filtration
  5. customThe obtained crystal was dried under reduced pressure

출처 및 근거

ORD 기록
ord-679fa92b90ec4298acc84370b9c1d365
출처 데이터셋
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08785631B2

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