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

HRID 441993노트

반응식

HRID 441993 반응식
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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-436c3896fa3c4dc7bdd06adaa752bb5a
출처 데이터셋
uspto-grants-1977_08
특허 번호
US04044010

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