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

HRID 2386667
ノート
印刷プレビュー

反応式

HRID 2386667 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-5b0ce1d5da474ef597cc81994819fb4a
出典データセット
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08268840B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート