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

HRID 1596216ノート

反応式

HRID 1596216 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-a5f6a829e6e14ff0b8e2c97bc765dc5d
出典データセット
uspto-grants-2001_09
特許番号
US06291464B1

反応ノート

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