Sodium Iodide → 1-{2-[4-(10,11-Dihydro-3-methoxy-8-methylthio-dibenzo[b,f]thiepin-10-yl)-1-piperazinyl]-ethyl}-2-pyrrolidinone

HRID 441991노트

반응식

HRID 441991 반응식
[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]2[CH2:12][CH:11]([N:13]3[CH2:18][CH2:17][NH:16][CH2:15][CH2:14]3)[C:10]3[CH:19]=[C:20]([S:23][CH3:24])[CH:21]=[CH:22][C:9]=3[S:8][C:7]=2[CH:25]=1.C(=O)([O-])[O-].[K+].[K+].[I-].[Na+].Cl[CH2:35][CH2:36][N:37]1[CH2:41][CH2:40][CH2:39][C:38]1=[O:42]>C1(C)C=CC=CC=1>[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]2[CH2:12][CH:11]([N:13]3[CH2:14][CH2:15][N:16]([CH2:35][CH2:36][N:37]4[CH2:41][CH2:40][CH2:39][C:38]4=[O:42])[CH2:17][CH2:18]3)[C:10]3[CH:19]=[C:20]([S:23][CH3:24])[CH:21]=[CH:22][C:9]=3[S:8][C:7]=2[CH:25]=1

참가 물질

6

반응물 4

HCID 5238Sodium IodideHCID 11430Potassium CarbonateHCID 31566501-(2-Chloroethyl)pyrrolidin-2-oneHCID 134982451-(10,11-Dihydro-3-methoxy-8-methylthio-dibenzo[b,f]thiepin-10-yl)-piperazine

생성물 1

HCID 214162011-{2-[4-(10,11-Dihydro-3-methoxy-8-methylthio-dibenzo[b,f]thiepin-10-yl)-1-piperazinyl]-ethyl}-2-pyrrolidinone

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

11 G. of 1-(10,11-dihydro-3-methoxy-8-methylthio-dibenzo[b,f]thiepin-10-yl)-piperazine are heated together with 15 g. of potassium carbonate, 0.5 g. of sodium iodide, 11 g. of N-( β-chloroethyl)-2-pyrrolidinone and 100 ml. of toluene under reflux conditions for 17 hours. Then, the mixture is evaporated under reduced pressure. The residue is partitioned between water and ether, and the ethereal phase dried over sodium sulfate and evaporated. The residue obtained is chromatographed with chloroform over aluminum oxide. The 1-{2-[4-(10,11-dihydro-3-methoxy-8-methylthio-dibenzo[b,f]thiepin-10-yl)-1-piperazinyl]-ethyl}-2-pyrrolidinone thus obtained is converted into the corresponding dihydrochloride by reaction with hydrogen chloride. The resulting dihydrochloride melts at 202° C.

후처리

  1. customThen, the mixture is evaporated under reduced pressure
  2. customThe residue is partitioned between water and ether
  3. dry with materialthe ethereal phase dried over sodium sulfate
  4. customevaporated
  5. customThe residue obtained
  6. customis chromatographed with chloroform over aluminum oxide

출처 및 근거

ORD 기록
ord-ee766f5d2b4348548babad1c88badeb1
출처 데이터셋
uspto-grants-1977_08
특허 번호
US04044010

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