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Hydrochloric Acid → 4-(Cyclopentylamino)-2-(methylthio)pyrimidine-5-carboxylic acid

HRID 2386667
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반응식

HRID 2386667 반응식
[OH-].[Na+].C([O:5][C:6]([C:8]1[C:9]([NH:16][CH:17]2[CH2:21][CH2:20][CH2:19][CH2:18]2)=[N:10][C:11]([S:14][CH3:15])=[N:12][CH:13]=1)=[O:7])C.Cl>CCO>[CH:17]1([NH:16][C:9]2[C:8]([C:6]([OH:7])=[O:5])=[CH:13][N:12]=[C:11]([S:14][CH3:15])[N:10]=2)[CH2:18][CH2:19][CH2:20][CH2:21]1
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참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 9151473Ethyl 4-(cyclopentylamino)-2-(methylsulfanyl)pyrimidine-5-carboxylate

생성물 1

HCID 223298834-(Cyclopentylamino)-2-(methylthio)pyrimidine-5-carboxylic acid수율 97.2%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

NaOH (1 M aq, 31 mL) was added to a suspension of 4-cyclopentylamino-2-methylsulfanyl-pyrimidine-5-carboxylic acid ethyl ester (11.7 g, 41.6 mmol) in EtOH (14 mL) and the resulting mixture was heated at reflux for 1.5 h. The reaction mixture was cooled to RT and HCl (1 M aq) was added until pH 4 was reached. The white solid, which crashed out of solution, was collected by filtration, washed with water and heptane and then dried under reduced pressure to afford 10.241 g (97% yield) of 4-cyclopentylamino-2-methylsulfanyl-pyrimidine-5-carboxylic acid.

후처리

  1. temperaturethe resulting mixture was heated
  2. temperatureat reflux for 1.5 h
  3. filtrationwas collected by filtration
  4. washwashed with water and heptane
  5. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-5b0ce1d5da474ef597cc81994819fb4a
출처 데이터셋
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08268840B2

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