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1-Piperazinecarboxylic acid, ethyl ester → 1-Carbethoxy-4-(8-chloro-2-methyl-dibenzo[b,f]thiepin-10-yl)-piperazine

HRID 441979
ノート
印刷プレビュー

反応式

HRID 441979 の反応式
[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][C:7](=O)[C:6]=2[CH:18]=1.[C:19]([N:24]1[CH2:29][CH2:28][NH:27][CH2:26][CH2:25]1)([O:21][CH2:22][CH3:23])=[O:20].C(=O)(O)[O-].[Na+]>[Ti](Cl)(Cl)(Cl)Cl.C1C=CC=CC=1>[C:19]([N:24]1[CH2:29][CH2:28][N:27]([C:7]2[C:6]3[CH:18]=[C:2]([Cl:1])[CH:3]=[CH:4][C:5]=3[S:11][C:10]3[CH:12]=[CH:13][C:14]([CH3:16])=[CH:15][C:9]=3[CH:8]=2)[CH2:26][CH2:25]1)([O:21][CH2:22][CH3:23])=[O:20]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 84311-Piperazinecarboxylic acid, ethyl esterHCID 516892Sodium BicarbonateHCID 214160928-chloro-2-methyl-dibenzo[b,f]thiepin-10(11H)-one

生成物 1

HCID 214161321-Carbethoxy-4-(8-chloro-2-methyl-dibenzo[b,f]thiepin-10-yl)-piperazine

試薬・触媒・溶媒 2

HCID 24193Titanium Tetrachloride触媒
HCID 241
Benzene
溶媒
2 回

実験手順

111.4 G. of 8-chloro-2-methyl-dibenzo[b,f]thiepin-10(11H)-one in 1 l. of absolute benzene are mixed together with 268 ml. of carbethoxypiperazine and within 1 hour at 20°-25° with a solution of 65 ml. of titanium tetrachloride in 500 ml. of absolute benzene. The resulting reaction mixture thereafter is heated under reflux conditions over a period of 20 hours. The reaction mixture is then poured over a mixture of 500 ml. of saturated aqueous sodium bicarbonate solution and 700 ml. of water with strong stirring, subsequently filtered, and washed again with chloroform. After an equilibrium is reached between both phases, the organic phase is dried and evaporated, whereby there is obtained 1-carbethoxy-4-(8-chloro-2-methyl-dibenzo[b,f]thiepin-10-yl)-piperazine as a dark brown viscous oil.

後処理

  1. customThe resulting reaction mixture
  2. temperaturethereafter is heated under reflux conditions over a period of 20 hours
  3. additionThe reaction mixture is then poured over a mixture of 500 ml
  4. filtrationof water with strong stirring, subsequently filtered
  5. washwashed again with chloroform
  6. customthe organic phase is dried
  7. customevaporated

出典と根拠

ORDレコード
ord-e02dae08cf284ece8132a1469e08e219
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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