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

HRID 737136
ノート
印刷プレビュー

反応式

HRID 737136 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>[C:31]1([NH:32][C:33]([N:13]2[CH2:12][CH2:11][N:10]([CH2:14][C:15]3[CH:20]=[CH:19][C:18]([C:21]4[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=4[C:27]([F:30])([F:28])[F:29])=[CH:17][CH:16]=3)[CH2:9][CH:8]2[CH2:1][C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)=[O:34])[CH:9]=[CH:8][CH:1]=[CH:2][CH:3]=1
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 690563552-Benzyl-4-(2'-trifluoromethyl-biphenyl-4-ylmethyl)-piperazine-1-carboxylic acid phenylamide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

The above compound was made in the following manner: 100 mg of 3-benzyl-1-(2′-trifluoromethyl-biphenyl-4-ylmethyl)-piperazine dissolved in dichloromethane, 1.1 equiv. methylisocyanate added. The reaction was shaken at room temperature overnight. The reaction was concentrated in vacuo. The residue was diluted with DCM, washed with 1M aqueous sodium hydroxide solution, then dried over sodium sulfate, filtered and concentrated in vacuo. The crude product was identified by ES MS(+) (m/z 530).

後処理

  1. concentrationThe reaction was concentrated in vacuo
  2. additionThe residue was diluted with DCM
  3. washwashed with 1M aqueous sodium hydroxide solution
  4. dry with materialdried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-f719f980ad9a47b19ef9fb21916a775a
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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