Potassium Iodide → 1-[2-[4-(2-Chloro-10,11-dihydro-dibenzo[b,f]thiepin-10-yl)-1-piperazinyl]-ethyl]-3-methyl-2-imidazolidinone

HRID 435647ノート

反応式

HRID 435647 の反応式
[Cl:1][C:2]1[CH:22]=[CH:21][C:5]2[S:6][C:7]3[CH:20]=[CH:19][CH:18]=[CH:17][C:8]=3[CH:9]([N:11]3[CH2:16][CH2:15][NH:14][CH2:13][CH2:12]3)[CH2:10][C:4]=2[CH:3]=1.C(=O)([O-])[O-].[K+].[K+].[I-].[K+].Cl[CH2:32][CH2:33][N:34]1[CH2:38][CH2:37][N:36]([CH3:39])[C:35]1=[O:40]>O.C1(C)C=CC=CC=1>[Cl:1][C:2]1[CH:22]=[CH:21][C:5]2[S:6][C:7]3[CH:20]=[CH:19][CH:18]=[CH:17][C:8]=3[CH:9]([N:11]3[CH2:12][CH2:13][N:14]([CH2:32][CH2:33][N:34]4[CH2:38][CH2:37][N:36]([CH3:39])[C:35]4=[O:40])[CH2:15][CH2:16]3)[CH2:10][C:4]=2[CH:3]=1

参加物

7

反応物 4

HCID 4875Potassium IodideHCID 11430Potassium CarbonateHCID 30559791-(3-Chloro-5,6-dihydrobenzo[b][1]benzothiepin-6-yl)piperazineHCID 156531101-(2-Chloroethyl)-3-methylimidazolidin-2-one

生成物 1

HCID 214811531-[2-[4-(2-Chloro-10,11-dihydro-dibenzo[b,f]thiepin-10-yl)-1-piperazinyl]-ethyl]-3-methyl-2-imidazolidinone

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 1140Toluene溶媒

実験手順

8.3 g of 1-(2-chloro-10,11-dihydro-dibenzo[b,f]thiepin-10-yl)-piperazine are treated, together with 11.6 g of powdered potassium carbonate, 0.2 g of potassium iodide and 80 ml of toluene, with 8.6 g of β-chloroethyl-3-methyl-2-imidazolidinone and the mixture is heated under reflux for 20 hours. The mixture is then poured into water, the organic phase washed with water, dried over sodium sulphate and evaporated. There is obtained 1-[2-[4-(2-chloro-10,11-dihydro-dibenzo[b,f]thiepin-10-yl)-1-piperazinyl]-ethyl]-3-methyl-2-imidazolidinone as a brown oil. By treatment of this compound with maleic acid in ethanol/ether there is obtained the corresponding maleate which melts at 186°-188° C.

後処理

  1. temperaturethe mixture is heated
  2. temperatureunder reflux for 20 hours
  3. washthe organic phase washed with water
  4. dry with materialdried over sodium sulphate
  5. customevaporated

出典と根拠

ORDレコード
ord-e7a1e78966c74566b1042a35d9ba637e
出典データセット
uspto-grants-1977_02
特許番号
US04006145

反応ノート

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