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3-[2-(1-Piperazinyl)ethyl]-2-oxazolidinone → 3-{2-[4-(8-Fluoro-10,11-dihydro-3-methyl-dibenzo[b,f]thiepin-10-yl)-1-piperazinyl]-ethyl}-2-oxazolidinone

HRID 441996
ノート
印刷プレビュー

反応式

HRID 441996 の反応式
Cl[CH:2]1[C:8]2[CH:9]=[C:10]([F:13])[CH:11]=[CH:12][C:7]=2[S:6][C:5]2[CH:14]=[C:15]([CH3:18])[CH:16]=[CH:17][C:4]=2[CH2:3]1.[N:19]1([CH2:25][CH2:26][N:27]2[CH2:31][CH2:30][O:29][C:28]2=[O:32])[CH2:24][CH2:23][NH:22][CH2:21][CH2:20]1>C(Cl)(Cl)Cl>[F:13][C:10]1[CH:11]=[CH:12][C:7]2[S:6][C:5]3[CH:14]=[C:15]([CH3:18])[CH:16]=[CH:17][C:4]=3[CH2:3][CH:2]([N:22]3[CH2:23][CH2:24][N:19]([CH2:25][CH2:26][N:27]4[CH2:31][CH2:30][O:29][C:28]4=[O:32])[CH2:20][CH2:21]3)[C:8]=2[CH:9]=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 2141615710-Chloro-8-fluoro-10,11-dihydro-3-methyldibenzo[b,f]thiepin

生成物 1

HCID 214162053-{2-[4-(8-Fluoro-10,11-dihydro-3-methyl-dibenzo[b,f]thiepin-10-yl)-1-piperazinyl]-ethyl}-2-oxazolidinone

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

10.6 g. of 10-chloro-8-fluoro-10,11-dihydro-3-methyl-dibenzo[b,f]thiepin are heated at reflux together with 200 ml. of chloroform and 22.8 g. of 3-[2-(1-piperazinyl)-ethyl]-2-oxazolidinone for 30 hours. Thereafter, the mixture is evaporated under reduced pressure, and the residue is worked up as described in Example 5. The insoluble base is recrystallized from ethanol, whereby there is obtained 3-{2-[4-(8-fluoro-10,11-dihydro-3-methyl-dibenzo[b,f]thiepin-10-yl)-1-piperazinyl]-ethyl}-2-oxazolidinone which melts at 173°-175° C. The maleate crystallizes from acetone/ether and has a melting point of 147°-149° C.

後処理

  1. temperatureat reflux together with 200 ml
  2. customThereafter, the mixture is evaporated under reduced pressure
  3. customThe insoluble base is recrystallized from ethanol

出典と根拠

ORDレコード
ord-4e6cf82ac527423f930f1a9735f88cc5
出典データセット
uspto-grants-1977_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04044010

反応ノート

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