Potassium Carbonate → HCID 20161923、化合物

HRID 247167ノート

反応式

HRID 247167 の反応式
C([NH:9][C:10]([NH:12][CH2:13][CH2:14][S:15][CH2:16][C:17]1[O:18][C:19]([CH2:22][N:23]([CH3:25])[CH3:24])=[CH:20][CH:21]=1)=[S:11])(=O)C1C=CC=CC=1.C(=O)([O-])[O-].[K+].[K+]>C(O)C.O>[CH3:25][N:23]([CH2:22][C:19]1[O:18][C:17]([CH2:16][S:15][CH2:14][CH2:13][NH:12][C:10]([NH2:9])=[S:11])=[CH:21][CH:20]=1)[CH3:24]

参加物

5

反応物 2

HCID 11430Potassium Carbonate2 回HCID 20161927HCID 20161927、化合物

生成物 1

HCID 20161923HCID 20161923、化合物

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

反応条件

温度
65 °C

実験手順

A mixture of 24.76 g (65.6 mmol) of N-benzoyl-N'-(2-(((5-(dimethylamino)methyl-2-furanyl)methyl)thio)ethyl)-thiourea and 5.6 g (40.5 mmol) of potassium carbonate in 160 ml ethanol and 100 ml water is heated under stirring at 65° C. An additional amount of 3.45 g (25 mmol) potassium carbonate is added after 30 and 75 minutes respectively. After 90 minutes the ethanol is eliminated by vacuum distillation. A reaction mixture is diluted with 200 ml 5% sodium carbonate and extracted with dichloromethane (3×250 ml). The organic compound is washed with 5% sodium carbonate (2×500 ml), dried over anhydrous magnesium sulfate and concentrated to a brown oil. After chromatography on 500 g silica gel in dichloromethane/methanol 9:1, 16.8 g of N-(2-(((5-(dimethylamino)methyl-2-furanyl)methyl)thio)ethyl-thiourea oil is obtained.

後処理

  1. temperatureis heated
  2. distillationAfter 90 minutes the ethanol is eliminated by vacuum distillation
  3. additionA reaction mixture is diluted with 200 ml 5% sodium carbonate
  4. extractionextracted with dichloromethane (3×250 ml)
  5. washThe organic compound is washed with 5% sodium carbonate (2×500 ml)
  6. dry with materialdried over anhydrous magnesium sulfate
  7. concentrationconcentrated to a brown oil

出典と根拠

ORDレコード
ord-81ba8e680d524eeab41b48dfe06b679a
出典データセット
uspto-grants-1987_11
特許番号
US04705873

反応ノート

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