Hydrochloric Acid → 1-Benzylpiperidine-4-acetonitrile

HRID 470626

반응식

HRID 470626 반응식
[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

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 5462224MagnesiumHCID 122015212-(1-Benzylpiperidin-4-ylidene)acetonitrile2회

생성물 1

HCID 5624991-Benzylpiperidine-4-acetonitrile

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-4aa1d79e9e7d4f9f8508f261759f8239
출처 데이터셋
uspto-grants-2014_01
특허 번호
US08629277B2

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