Methanol → (S)-1-Acetyl-2-methyl-4-benzylpiperazine

HRID 1596216노트

반응식

HRID 1596216 반응식
[CH2:1]([N:8]1[CH2:13][CH2:12][NH:11][C@@H:10]([CH3:14])[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(N(CC)CC)C.[C:22](OC(=O)C)(=[O:24])[CH3:23].CO>ClCCl>[C:22]([N:11]1[CH2:12][CH2:13][N:8]([CH2:1][C:2]2[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=2)[CH2:9][C@@H:10]1[CH3:14])(=[O:24])[CH3:23]

참가 물질

6

반응물 4

HCID 887MethanolHCID 7918Acetic AnhydrideHCID 8471TriethylamineHCID 6923224(S)-1-Benzyl-3-methylpiperazine

생성물 1

HCID 54471759(S)-1-Acetyl-2-methyl-4-benzylpiperazine

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a stirred solution of (S)-1-benzyl-3-methylpiperazine (588 mg) and triethylamine (0.47 ml) in dichloromethane (5 ml) was added acetic anhydride (0.32 ml) at 0° C. The reaction mixture was stirred at ambient temperature for 4 hours. Methanol was added to this solution and evaporated. The residue was taken up in ethyl acetate and washed with water and brine. The organic layer was dried over magnesium sulfate and concentrated. The residue was purified by column chromatography eluting with a mixture of ethyl acetate and n-hexane (2:1) to give (S)-1-acetyl-4-benzyl-2-methylpiperazine (660 mg).

후처리

  1. customevaporated
  2. washwashed with water and brine
  3. dry with materialThe organic layer was dried over magnesium sulfate
  4. concentrationconcentrated
  5. customThe residue was purified by column chromatography
  6. washeluting with a mixture of ethyl acetate and n-hexane (2:1)

출처 및 근거

ORD 기록
ord-a5f6a829e6e14ff0b8e2c97bc765dc5d
출처 데이터셋
uspto-grants-2001_09
특허 번호
US06291464B1

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