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Hydrochloric Acid → 2,6-dimethyl-3-piperidin-4-yl-3H-imidazo[4,5-c]pyridine

HRID 1716603
ノート
印刷プレビュー

反応式

HRID 1716603 の反応式
[CH3:1][C:2]1[N:11]([CH:12]2[CH2:17][CH2:16][N:15](C(=O)C)[CH2:14][CH2:13]2)[C:5]2[CH:6]=[N:7][C:8]([CH3:10])=[CH:9][C:4]=2[N:3]=1.Cl>C(O)C>[CH3:1][C:2]1[N:11]([CH:12]2[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]2)[C:5]2[CH:6]=[N:7][C:8]([CH3:10])=[CH:9][C:4]=2[N:3]=1
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 685145831-[4-(2,6-Dimethyl-imidazo[4,5-c]-pyridin-3-yl)-piperidin-1-yl]-ethanone

生成物 1

HCID 588522922,6-dimethyl-3-piperidin-4-yl-3H-imidazo[4,5-c]pyridine収率 77%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
100 °C

実験手順

A solution of 1-[4-(2,6-dimethyl-imidazo[4,5-c]-pyridin-3-yl)-piperidin-1-yl]-ethanone) 20 mg, 0.0735 mmol) in ethanol (0.5 mL) was treated with concentrated HCl (0.5 mL). The reaction mixture was heated at 100° C. for 18 h. The solvent was evaporated and the mixture was diluted with water (2 mL). The mixture was washed with diethyl ether and the aqueous phase was adjusted to pH=10 by addition of a solution of 25% aqueous NaOH. The aqueous mixture was extracted with CH2Cl2 (5×10 mL). The combined extracts were washed with brine, dried over anhydrous Na2SO4, filtered and concentrated in vacuo to afford 2,6-dimethyl-3-piperidin-4-yl-3H-imidazo[4,5-c]pyridine (13 mg, 77%) as a light yellow solid which was used without further purification.

後処理

  1. customThe solvent was evaporated
  2. additionthe mixture was diluted with water (2 mL)
  3. washThe mixture was washed with diethyl ether
  4. additionthe aqueous phase was adjusted to pH=10 by addition of a solution of 25% aqueous NaOH
  5. extractionThe aqueous mixture was extracted with CH2Cl2 (5×10 mL)
  6. washThe combined extracts were washed with brine
  7. dry with materialdried over anhydrous Na2SO4
  8. filtrationfiltered
  9. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-9156f7693b684510afab1fd0d5f13729
出典データセット
uspto-grants-2010_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07803816B2

反応ノート

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