Sodium Carbonate → Methyl 4-(2-methylthiobenzyl)-1-piperazinecarbodithioate

HRID 1757557ノート

反応式

HRID 1757557 の反応式
[CH3:1][S:2][C:3]1[CH:10]=[CH:9][CH:8]=[CH:7][C:4]=1[CH2:5]Cl.[N:11]1([C:17]([S:19][CH3:20])=[S:18])[CH2:16][CH2:15][NH:14][CH2:13][CH2:12]1.C(=O)([O-])[O-].[Na+].[Na+]>C(O)C>[CH3:1][S:2][C:3]1[CH:10]=[CH:9][CH:8]=[CH:7][C:4]=1[CH2:5][N:14]1[CH2:15][CH2:16][N:11]([C:17]([S:19][CH3:20])=[S:18])[CH2:12][CH2:13]1

参加物

5

反応物 3

HCID 10340Sodium CarbonateHCID 124145821-(Chloromethyl)-2-(methylsulfanyl)benzeneHCID 21278808Methyl piperazine-1-carbodithioate

生成物 1

HCID 19388454Methyl 4-(2-methylthiobenzyl)-1-piperazinecarbodithioate収率 31%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

In 20 ml of ethanol, 2.1 g (12.2 mmol.) of 2-methylthiobenzyl chloride, 2.17 g (12.3 mmol.) of methyl 1-piperazinecarbodithioate and 1.30 g (12.3 mmol.) of sodium carbonate were refluxed under heating for 2 hours. Ethanol was distilled off under reduced pressure. The residue was extracted with ether, after addition of water. The ether portion was washed with water and a saturated aqueous sodium chloride solution, dried over anhydrous sodium sulfate, and placed under reduced pressure to distill off the solvent. The residue was purified over silica gel column, to give 1.18 g of the desired compound as a yellow oil, yield 31%.

後処理

  1. temperatureunder heating for 2 hours
  2. distillationEthanol was distilled off under reduced pressure
  3. extractionThe residue was extracted with ether
  4. additionafter addition of water
  5. washThe ether portion was washed with water
  6. dry with materiala saturated aqueous sodium chloride solution, dried over anhydrous sodium sulfate
  7. distillationto distill off the solvent
  8. customThe residue was purified over silica gel column

出典と根拠

ORDレコード
ord-729dfe6b62254b40b5820ac69f7072bd
出典データセット
uspto-grants-1995_08
特許番号
US05446146

反応ノート

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