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Methyl Isocyanate → 2-Benzyl-4-(2'-trifluoromethyl-biphenyl-4-ylmethyl)-piperazine-1-carboxylic acid methylamide

HRID 737135
ノート
印刷プレビュー

反応式

HRID 737135 の反応式
[CH2:1]([CH:8]1[NH:13][CH2:12][CH2:11][N:10]([CH2:14][C:15]2[CH:20]=[CH:19][C:18]([C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=3[C:27]([F:30])([F:29])[F:28])=[CH:17][CH:16]=2)[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH3:31][N:32]=[C:33]=[O:34]>ClCCl>[CH3:31][NH:32][C:33]([N:13]1[CH2:12][CH2:11][N:10]([CH2:14][C:15]2[CH:20]=[CH:19][C:18]([C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=3[C:27]([F:30])([F:28])[F:29])=[CH:17][CH:16]=2)[CH2:9][CH:8]1[CH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1)=[O:34]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 12228Methyl IsocyanateHCID 235851083-Benzyl-1-(2'-trifluoromethyl-biphenyl-4-ylmethyl)-piperazine

生成物 1

HCID 578495812-Benzyl-4-(2'-trifluoromethyl-biphenyl-4-ylmethyl)-piperazine-1-carboxylic acid methylamide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

This compound could be made in the following manner: 100 mg of 3-benzyl-1-(2′-trifluoromethyl-biphenyl-4-ylmethyl)-piperazine would be dissolved in dichloromethane, 1.1 equiv. methylisocyanate would be added. The reaction would be shaken at room temperature overnight. The reaction would be concentrated in vacuo. The residue would be diluted with DCM, washed with 1M aqueous sodium hydroxide solution, then dried over sodium sulfate, filtered and concentrated in vacuo. The crude residue would be purified by column chromatography to afford the title compound as free base. Addition of 1 equiv. of 1M HCl in dioxane and concentratation in vacuo would afford the title compound as hydrochloride salt.

後処理

  1. customThe reaction
  2. customThe reaction
  3. concentrationwould be concentrated in vacuo
  4. additionThe residue would be diluted with DCM
  5. washwashed with 1M aqueous sodium hydroxide solution
  6. dry with materialdried over sodium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo
  9. customThe crude residue would be purified by column chromatography

出典と根拠

ORDレコード
ord-3a9a2acb0df54b3e9479a48e6cdb0809
出典データセット
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07595397B2

反応ノート

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