Ethylene Glycol → 1-(10,11-Dihydro-3-methoxy-8-methylthio-dibenzo[b,f]thiepin-10-yl)-piperazine

HRID 441993ノート

反応式

HRID 441993 の反応式
C([N:6]1[CH2:11][CH2:10][N:9]([CH:12]2[C:18]3[CH:19]=[C:20]([S:23][CH3:24])[CH:21]=[CH:22][C:17]=3[S:16][C:15]3[CH:25]=[C:26]([O:29][CH3:30])[CH:27]=[CH:28][C:14]=3[CH2:13]2)[CH2:8][CH2:7]1)(OCC)=O.C(O)CO.[OH-].[K+]>O>[CH3:30][O:29][C:26]1[CH:27]=[CH:28][C:14]2[CH2:13][CH:12]([N:9]3[CH2:8][CH2:7][NH:6][CH2:11][CH2:10]3)[C:18]3[CH:19]=[C:20]([S:23][CH3:24])[CH:21]=[CH:22][C:17]=3[S:16][C:15]=2[CH:25]=1

参加物

5

反応物 3

HCID 174Ethylene GlycolHCID 14797Potassium HydroxideHCID 134982441-Carbethoxy-4-(10,11-dihydro-3-methoxy-8-methylthio-dibenzo[b,f]thiepin-10-yl)-piperazine

生成物 1

HCID 134982451-(10,11-Dihydro-3-methoxy-8-methylthio-dibenzo[b,f]thiepin-10-yl)-piperazine

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

61 G. of 1-carbethoxy-4-(10,11-dihydro-3-methoxy-8-methylthio-dibenzo[b,f]thiepin-10-yl)-piperazine, 600 ml. of ethylene glycol, 25 g. of potassium hydroxide and 2.7 ml. of water are heated at 160° C. for a period of 2 hours. Then, the mixture is poured on to water and extracted with benzene. The organic phase is washed with water, dried over magnesium sulfate and evaporated under reduced pressure, whereby there is obtained 1-(10,11-dihydro-3-methoxy-8-methylthio-dibenzo[b,f]thiepin-10-yl)-piperazine.

後処理

  1. extractionextracted with benzene
  2. washThe organic phase is washed with water
  3. dry with materialdried over magnesium sulfate
  4. customevaporated under reduced pressure

出典と根拠

ORDレコード
ord-436c3896fa3c4dc7bdd06adaa752bb5a
出典データセット
uspto-grants-1977_08
特許番号
US04044010

反応ノート

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