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Sodium Iodide → 1-{2-[4-(8-Chloro-10,11-dihydro-2-methyl-dibenzo[b,f]thiepin-10-yl)1-piperazinyl]-ethyl}-2-pyrrolidinone

HRID 441978
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HRID 441978 반응식
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[S:11][C:10]3[CH:12]=[CH:13][C:14]([CH3:16])=[CH:15][C:9]=3[CH2:8][CH:7]([N:17]3[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]3)[C:6]=2[CH:23]=1.C(=O)([O-])[O-].[K+].[K+].[I-].[Na+].Cl[CH2:33][CH2:34][N:35]1[CH2:39][CH2:38][CH2:37][C:36]1=[O:40]>C1(C)C=CC=CC=1>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[S:11][C:10]3[CH:12]=[CH:13][C:14]([CH3:16])=[CH:15][C:9]=3[CH2:8][CH:7]([N:17]3[CH2:22][CH2:21][N:20]([CH2:33][CH2:34][N:35]4[CH2:39][CH2:38][CH2:37][C:36]4=[O:40])[CH2:19][CH2:18]3)[C:6]=2[CH:23]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 5238Sodium IodideHCID 11430Potassium CarbonateHCID 31566501-(2-Chloroethyl)pyrrolidin-2-oneHCID 214161631-(8-Chloro-10,11-dihydro-2-methyl-dibenzo[b,f]thiepin-10-yl)piperazine

생성물 1

HCID 214161651-{2-[4-(8-Chloro-10,11-dihydro-2-methyl-dibenzo[b,f]thiepin-10-yl)1-piperazinyl]-ethyl}-2-pyrrolidinone

시약·촉매·용매 1

HCID 1140
Toluene
용매

실험 절차

11 G. of 1-(8-chloro-10,11-dihydro-2-methyl-dibenzo[b,f]thiepin-10-yl)piperazine are heated together with 15.5 g. of potassium carbonate, 0.5 g. of sodium iodide, 11 g. of N-(beta-chloroethyl)-pyrrolidinone and 150 ml. of toluene under reflux conditions over a period of 12 hours. The reaction mixture is evaporated under reduced pressure. The residue is dispersed between water and ether and the ethereal phase is dried over sodium sulfate and evaporated, whereby there is obtained 1-{-2-[4-(8-chloro-10,11-dihydro-2-methyl-dibenzo[b,f]thiepin10-yl)-1-piperazinyl]-ethyl}-2-pyrrolidinone, having a melting point of 153°-164°. The maleate melts at 179°-180°.

후처리

  1. customThe reaction mixture is evaporated under reduced pressure
  2. additionThe residue is dispersed between water and ether
  3. dry with materialthe ethereal phase is dried over sodium sulfate
  4. customevaporated

출처 및 근거

ORD 기록
ord-42eeaf7efd464af4bd758a1d694110be
출처 데이터셋
uspto-grants-1977_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04044010

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