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Hydrochloric Acid → (S)-N-methyl-N-(piperidin-3-yl)-1H-pyrazolo[3,4-d]pyrimidin-4-amine

HRID 919558
ノート
印刷プレビュー

反応式

HRID 919558 の反応式
[CH3:1][N:2]([C@H:20]1[CH2:25][CH2:24][CH2:23][NH:22][CH2:21]1)[C:3]1[N:8]=[CH:7][N:6]=[C:5]2[N:9](COCC[Si](C)(C)C)[N:10]=[CH:11][C:4]=12.Cl>CCO>[CH3:1][N:2]([C@H:20]1[CH2:25][CH2:24][CH2:23][NH:22][CH2:21]1)[C:3]1[N:8]=[CH:7][N:6]=[C:5]2[NH:9][N:10]=[CH:11][C:4]=12
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 86706439(S)-N-methyl-N-(piperidin-3-yl)-1-((2-(trimethylsilyl)ethoxy)methyl)-1H-pyrazolo[3,4-d]pyrimidin-4-amine

生成物 1

HCID 118906718(S)-N-methyl-N-(piperidin-3-yl)-1H-pyrazolo[3,4-d]pyrimidin-4-amine収率 95.7%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
60 °C

実験手順

To a solution of (S)—N-methyl-N-(piperidin-3-yl)-1-((2-(trimethylsilyl)ethoxy)methyl)-1H-pyrazolo[3,4-d]pyrimidin-4-amine (310 mg, 0.85 mmol) in EtOH (7.5 mL), cone. HCl (2.5 mL) was added and the reaction mixture was heated at 60° C. for 5 h. The reaction mixture was concentrated in vacuo and the residue was dissolved in MeOH (5 mL) and a polymer support carbonate resin was added until the mixture turned basic (Checked by litmus paper). The reaction mixture was filtered and the filtrate was concentrated in vacuo to yield the titled intermediate (189 mg, 95%), which was used further without further purification. LC-MS: m/z [M+1]=233.

後処理

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. dissolutionthe residue was dissolved in MeOH (5 mL)
  3. additiona polymer support carbonate resin was added until the mixture
  4. filtrationThe reaction mixture was filtered
  5. concentrationthe filtrate was concentrated in vacuo

出典と根拠

ORDレコード
ord-eb2a273a7a8b4b1ca8700bcbe185b0bc
出典データセット
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09273028B2

反応ノート

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