Hydrochloric Acid → 1-Benzylpiperidine-4-acetonitrile

HRID 470626

反応式

HRID 470626 の反応式
[CH2:1]([N:8]1[CH2:13][CH2:12][C:11](=[CH:14][C:15]#[N:16])[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[Mg].Cl.[OH-].[Na+]>CO>[CH2:1]([N:8]1[CH2:13][CH2:12][CH:11]([CH2:14][C:15]#[N:16])[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 5462224MagnesiumHCID 122015212-(1-Benzylpiperidin-4-ylidene)acetonitrile2 回

生成物 1

HCID 5624991-Benzylpiperidine-4-acetonitrile

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of benzylpiperidin-4-ylideneacetonitrile (compound of Example 26; 1 g, 4.7 mmol) in methanol (50 mL), magnesium turnings (4.58 g, 188.3 mmol) was added at 0° C. The reaction mixture was stirred at 5° C. to 10° C. for 4 h. The magnesium salts were dissolved by addition of concentrated hydrochloric acid, and the mixture was basified with 10N sodium hydroxide solution. The precipitate was filtered and extracted with ethyl acetate (2×20 mL). The combined organic layers were washed with water (2×15 mL) followed by brine (10 mL). The organic phase obtained was dried over anhydrous sodium sulphate and evaporated to afford the title compound.

後処理

  1. filtrationThe precipitate was filtered
  2. extractionextracted with ethyl acetate (2×20 mL)
  3. washThe combined organic layers were washed with water (2×15 mL)
  4. customThe organic phase obtained
  5. dry with materialwas dried over anhydrous sodium sulphate
  6. customevaporated

出典と根拠

ORDレコード
ord-4aa1d79e9e7d4f9f8508f261759f8239
出典データセット
uspto-grants-2014_01
特許番号
US08629277B2

関連ノート

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