Hydrochloric Acid → Piperidine-4-carboxylic acid [6-(2-methoxy-phenyl)-pyrimidin-4-yl]-amide hydrochloride

HRID 1020050ノート

反応式

HRID 1020050 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[C:9]1[N:14]=[CH:13][N:12]=[C:11]([NH:15][C:16]([CH:18]2[CH2:23][CH2:22][NH:21][CH2:20][CH2:19]2)=[O:17])[CH:10]=1.[ClH:24]>O1CCOCC1>[ClH:24].[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[C:9]1[N:14]=[CH:13][N:12]=[C:11]([NH:15][C:16]([CH:18]2[CH2:23][CH2:22][NH:21][CH2:20][CH2:19]2)=[O:17])[CH:10]=1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 59508946Piperidine-4-carboxylic acid [6-(2-methoxy-phenyl)-pyrimidin-4-yl]amide

生成物 1

HCID 67184524Piperidine-4-carboxylic acid [6-(2-methoxy-phenyl)-pyrimidin-4-yl]-amide hydrochloride

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

Piperidine-4-carboxylic acid [6-(2-methoxy-phenyl)-pyrimidin-4-yl]amide (compound #6A) (2.0 g, 6.4 mmol) was dissolved in a saturated solution of HCl in 1,4-dioxane (50 ml) and the clear solution was stirred at room temperature for half an hour. A pale yellow solid precipitated out. Diethyl ether (50 ml) was added to precipitate more of the solid. After filtration, the solid was washed with diethyl ether (50 ml) and dried under high vacuum to obtain piperidine-4-carboxylic acid [6-(2-methoxy-phenyl)-pyrimidin-4-yl]-amide hydrochloride (compound #14A, HCl salt of compound #6A), 2.2 g, 98%) as a white solid.

後処理

  1. customA pale yellow solid precipitated out
  2. additionDiethyl ether (50 ml) was added
  3. customto precipitate more of the solid
  4. filtrationAfter filtration
  5. washthe solid was washed with diethyl ether (50 ml)
  6. customdried under high vacuum

出典と根拠

ORDレコード
ord-456c0ffd3ce74494b385458eda4ab5fc
出典データセット
uspto-grants-2014_05
特許番号
US08716296B2

反応ノート

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