Acetic Acid → HCID 22278860, 화합물

HRID 1063320노트

반응식

HRID 1063320 반응식
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

참가 물질

6

반응물 4

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

생성물 1

HCID 22278860HCID 22278860, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-0dda48a3488b4bb79b2a0430ee1a45a0
출처 데이터셋
uspto-grants-2005_11
특허 번호
US06964966B2

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