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4-(2-Trifluoromethylthiobenzoyl)piperazine-1-carboxylic acid tert-butyl ester → Methanethione, 1-piperazinyl[2-(trifluoromethyl)phenyl]-

HRID 2356590
ノート
印刷プレビュー

反応式

HRID 2356590 の反応式
C(OC([N:8]1[CH2:13][CH2:12][N:11]([C:14](=[S:25])[C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=2[C:21]([F:24])([F:23])[F:22])[CH2:10][CH2:9]1)=O)(C)(C)C>ClCCl.FC(F)(F)C(O)=O>[N:11]1([C:14]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=2[C:21]([F:24])([F:22])[F:23])=[S:25])[CH2:12][CH2:13][NH:8][CH2:9][CH2:10]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 1

HCID 865972314-(2-Trifluoromethylthiobenzoyl)piperazine-1-carboxylic acid tert-butyl ester

生成物 1

HCID 86025958Methanethione, 1-piperazinyl[2-(trifluoromethyl)phenyl]-収率 95.5%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 6422Trifluoroacetic acid溶媒

実験手順

A solution of 4-(2-trifluoromethylthiobenzoyl)piperazine-1-carboxylic acid tert-butyl ester (2.1 g, 5.61 mmol) in dichloromethane and trifluoroacetic acid (30 mL, 2:1) was stirred at ambient temperature overnight, the solvents were removed by evaporation. The residue was dissolved in ethyl acetate, and washed with aqueous saturated NaHCO3 and brine, dried over anhydrous Na2SO4 and concentrated to give piperazin-1-yl-(2-trifluoromethylphenyl)methanethione (1.47 g, 5.36 mmol) which was used directly for next step without further purification.

後処理

  1. customthe solvents were removed by evaporation
  2. dissolutionThe residue was dissolved in ethyl acetate
  3. washwashed with aqueous saturated NaHCO3 and brine
  4. dry with materialdried over anhydrous Na2SO4
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-4461ff68b5bb4ccbb9b78fa6bf65d3a9
出典データセット
uspto-grants-2010_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07759348B2

反応ノート

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