Acetic Acid → HCID 22278860、化合物

HRID 1063320ノート

反応式

HRID 1063320 の反応式
C=O.N[CH:4]1[CH2:9][CH2:8][N:7]([CH2:10][C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[CH2:6][C:5]1([CH2:18][CH3:19])[CH3:17].[C:20]([BH3-])#[N:21].[Na+].[C:24](O)(=O)C>CO>[CH2:10]([N:7]1[CH2:8][CH2:9][CH:4]([N:21]([CH3:20])[CH3:24])[C:5]([CH2:18][CH3:19])([CH3:17])[CH2:6]1)[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1

参加物

6

反応物 4

HCID 176Acetic AcidHCID 712FormaldehydeHCID 5003444Sodium cyanoborohydrideHCID 222788954-Amino-1-benzyl-3-ethyl-3-methylpiperidine

生成物 1

HCID 22278860HCID 22278860、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Paraformaldehyde (10 g) was added to the stirred solution of 4-amino-1-benzyl-3-ethyl-3-methylpiperidine (8.0 g, 34 mmol) in methanol (100 ml) at 0° C. and sodium cyanoborohydride (2.14 g, 34 mmol) was added to it. Then, acetic acid (2 ml) was added to the resulting mixture and stirring was continued for 24 hr at ambient temperature. The reaction mixture was concentrated to dryness, triturated with water, acidified with conc. HCl (pH 3˜4) and extracted with ethyl acetate to remove impurities. The aqueous layer was basified with 1 M sodium hydroxide solution (pH˜10) and extracted with ethyl acetate. Ethyl acetate extract was dried (Na2SO4) and concentrated to give 1-benzyl-4-dimethylamino-3-ethyl-3-methylpiperidine. Yield 6 g (67%), C17H28N2, m/z 261 (M+1).

後処理

  1. concentrationThe reaction mixture was concentrated to dryness
  2. customtriturated with water
  3. extractionextracted with ethyl acetate
  4. customto remove impurities
  5. extractionextracted with ethyl acetate
  6. extractionEthyl acetate extract
  7. dry with materialwas dried (Na2SO4)
  8. concentrationconcentrated

出典と根拠

ORDレコード
ord-0dda48a3488b4bb79b2a0430ee1a45a0
出典データセット
uspto-grants-2005_11
特許番号
US06964966B2

反応ノート

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