Trityl chloride → (S)-4-N-Trityl-2-methyl-piperazine

HRID 38295

反応式

HRID 38295 の反応式
[CH3:1][CH:2]1[CH2:7][NH:6][CH2:5][CH2:4][NH:3]1.C(N(CC)CC)C.[C:15](Cl)([C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1)([C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1)[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1>C(#N)C.C(Cl)Cl>[CH3:1][C@@H:2]1[NH:3][CH2:4][CH2:5][N:6]([C:15]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)([C:28]2[CH:29]=[CH:30][CH:31]=[CH:32][CH:33]=2)[C:22]2[CH:23]=[CH:24][CH:25]=[CH:26][CH:27]=2)[CH2:7]1

参加物

6

反応物 3

HCID 6456Trityl chlorideHCID 8471TriethylamineHCID 660572-Methylpiperazine

生成物 1

HCID 7171814(S)-4-N-Trityl-2-methyl-piperazine

試薬・触媒・溶媒 2

HCID 6342Acetonitrile溶媒HCID 6344Dichloromethane溶媒

実験手順

(S)+-2-methylpiperazine (10 g) was dissolved in acetonitrile (140 ml) and cooled to 5-10° C. whereupon triethylamine (35 ml) was added, followed by drop wise addition of a solution of trityl chloride 27.9 (g) in DCM (80 ml). The reaction was stirred for 1 h at room temperature. The resulting slurry was cooled to approximately 0° C. then filtered. The filtrate was evaporated in vacuo and the residue was purified by chromatography (silica, 1-4% MeOH/DCM as eluent) to give the sub-title compound (29 g).

後処理

  1. additionwas added
  2. temperatureThe resulting slurry was cooled to approximately 0° C.
  3. filtrationthen filtered
  4. customThe filtrate was evaporated in vacuo
  5. customthe residue was purified by chromatography (silica, 1-4% MeOH/DCM as eluent)

出典と根拠

ORDレコード
ord-3a98d504e8e4451b97bff5363160ad09
出典データセット
uspto-grants-2013_09
特許番号
US08524715B2

関連ノート

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