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3-[2-(1-Piperazinyl)ethyl]-2-oxazolidinone → HCID 21481136、化合物

HRID 435711
ノート
印刷プレビュー

反応式

HRID 435711 の反応式
Cl[CH:2]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[S:6][C:5]2[CH:13]=[CH:14][C:15]([C:17]([F:20])([F:19])[F:18])=[CH:16][C:4]=2[CH2:3]1.[N:21]1([CH2:27][CH2:28][N:29]2[CH2:33][CH2:32][O:31][C:30]2=[O:34])[CH2:26][CH2:25][NH:24][CH2:23][CH2:22]1>C(Cl)(Cl)Cl>[F:18][C:17]([F:20])([F:19])[C:15]1[CH:14]=[CH:13][C:5]2[S:6][C:7]3[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=3[CH:2]([N:24]3[CH2:25][CH2:26][N:21]([CH2:27][CH2:28][N:29]4[CH2:33][CH2:32][O:31][C:30]4=[O:34])[CH2:22][CH2:23]3)[CH2:3][C:4]=2[CH:16]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 122755453-[2-(1-Piperazinyl)ethyl]-2-oxazolidinoneHCID 15619006HCID 15619006、化合物

生成物 1

HCID 21481136HCID 21481136、化合物

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

17 g of 10-chloro-10,11-dihydro-2-trifluoromethyl-dibenzo[b,f]thiepin in 90 ml of chloroform and 26.2 g of 3-[2-(1-piperazinyl)-ethyl]-2-oxazolidinone are heated under reflux for 14 hours. The mixture is evaporated and the residue treated with ice-water, ether and 2-N aqueous sodium hydroxide. After equilibration, the organic phase is washed with water and acidified with ethanolic hydrochloric acid. The precipitate which separates is filtered off and dissolved in about 400 ml of water. The aqueous solution is extracted with ether. The aqueous solution is treated with ice, made alkaline with aqueous sodium hydroxide solution and extracted with about 350 ml of benzene. The benzene phase is dried over sodium sulphate, filtered and evaporated. There is obtained 3-[2-[4-(10,11-dihydro-2-trifluoromethyl-dibenzo[b,f]thiepin-10-yl)-1-piperazinyl]-ethyl]-2 -oxazolidinone as an oil. By treatment with maleic acid there is obtained the corresponding maleate which is crystallised from ethanol/ether; melting point 168°-169° C.

後処理

  1. temperatureunder reflux for 14 hours
  2. customThe mixture is evaporated
  3. additionthe residue treated with ice-water, ether and 2-N aqueous sodium hydroxide
  4. washAfter equilibration, the organic phase is washed with water
  5. filtrationThe precipitate which separates is filtered off
  6. dissolutiondissolved in about 400 ml of water
  7. extractionThe aqueous solution is extracted with ether
  8. additionThe aqueous solution is treated with ice
  9. extractionextracted with about 350 ml of benzene
  10. dry with materialThe benzene phase is dried over sodium sulphate
  11. filtrationfiltered
  12. customevaporated

出典と根拠

ORDレコード
ord-ae0fd6ea51454fda822ba22c7181a107
出典データセット
uspto-grants-1977_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04006144

反応ノート

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