Ethanol → Benzyl Diethyldithiocarbamate

HRID 2068460

反応式

HRID 2068460 の反応式
C(O)C.[CH2:4](Cl)[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1.O.O.O.[CH2:15]([N:17]([CH2:21][CH3:22])[C:18](=[S:20])[S-:19])[CH3:16].[Na+]>O>[CH2:15]([N:17]([CH2:21][CH3:22])[C:18](=[S:19])[S:20][CH2:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)[CH3:16]

参加物

5

反応物 3

HCID 702Ethanol2 回HCID 7503Benzyl ChlorideHCID 517546Sodium diethyldithiocarbamate trihydrate

生成物 1

HCID 590455Benzyl Diethyldithiocarbamate収率 93%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

More specifically, 10 ml of ethanol solution containing benzyl chloride (4.8 g, 38 mmol, Mw. 126.58) was added dropwise into 50 ml of ethanol solution containing sodium N,N-diethyldithiocarbamate trihydrate (10.3 g, 46 mmol, Mw. 225.31) in nitrogen atmosphere at 0° C. After agitating the reaction solution for 23 hours at room temperature, 150 ml of water was added and extracted by diethylether (200 ml×3 times). The organic layer was washed with water (100 ml×3 times) and was dried by sodium sulfate. Solvent was distilled away under reduced pressure using an evaporator so as to obtain benzyl N,N-diethyldithiocarbamate (colorless liquid). Yield point was 17.6 g (yield: 93%), 1H-NMR: δ7.407 ppm to 7.271 ppm (m, 5H, Ar—H), δ4.540 ppm (s, 2H, Ar—CH2S), δ4.082 ppm to 4.012 ppm (q, 2H, —N—CH2—), δ3.763 ppm to 3.692 ppm (q, 2H, —N—CH2—), δ1.311 to 1.252 ppm (m, 6H, —CH2—CH3).

後処理

  1. extractionextracted by diethylether (200 ml×3 times)
  2. washThe organic layer was washed with water (100 ml×3 times)
  3. dry with materialwas dried by sodium sulfate
  4. distillationSolvent was distilled away under reduced pressure
  5. customan evaporator so as

出典と根拠

ORDレコード
ord-ecacbc7fc529422db6b9a6f0cca9eaca
出典データセット
uspto-grants-2012_10
特許番号
US08298817B2

関連ノート

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