Hydrochloric Acid → HCID 54363196、化合物

HRID 259070

反応式

HRID 259070 の反応式
[CH3:1][C@H:2]1[CH2:7][NH:6][CH2:5][C@@H:4]([CH3:8])[NH:3]1.C1C=CC2S(=O)(=O)OC(C3C=C(Br)C(O)=C(Br)C=3)(C3C=C(Br)C(O)=C(Br)C=3)C=2C=1.Cl.Cl[C:40]([O:42][CH2:43][CH3:44])=[O:41].[OH-].[Na+].N1CCNCC1>O>[CH2:43]([O:42][C:40]([N:6]1[CH2:5][C@H:4]([CH3:8])[NH:3][C@H:2]([CH3:1])[CH2:7]1)=[O:41])[CH3:44]

参加物

8

反応物 6

HCID 313Hydrochloric AcidHCID 4837PiperazineHCID 8272Bromophenol Blue2 回HCID 10928Ethyl chloroformateHCID 14798Sodium Hydroxide2 回HCID 6950261rel-(2R,6S)-2,6-dimethylpiperazine

生成物 1

HCID 54363196HCID 54363196、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

To a solution of 50 grams of cis-2,6-dimethylpiperazine in 130 ml. of water and containing bromphenol blue as indicator is added, with stirring and cooling, a solution of 100 ml. of concentrated hydrochloric acid in 500 ml. of water until the bromphenol blue just turns yellow. Then, 47.7 grams of ethyl chloroformate is introduced in 5 ml. portions of rapid, dropwise addition with stirring. After each 5 ml. addition, aqueous 25% sodium hydroxide solution is added dropwise until the indicator turns green. The addition of reactants is continued until thin layer chromatography shows that all of the piperazine has reacted. The reaction mixture is then made alkaline with aqueous 50% sodium hydroxide solution and then extracted with ethyl ether. The combined ether extracts are dried over anhydrous sodium sulfate and then chromatographed to give 1-ethoxycarbonyl-cis-3,5-dimethylpiperazine.

後処理

  1. additionis added
  2. temperaturecooling
  3. additionportions of rapid, dropwise addition
  4. stirringwith stirring
  5. additionis added dropwise until the indicator
  6. additionThe addition of reactants
  7. customhas reacted
  8. extractionextracted with ethyl ether
  9. dry with materialThe combined ether extracts are dried over anhydrous sodium sulfate
  10. customchromatographed

出典と根拠

ORDレコード
ord-a7f3df1cf4454db2a03095ad2d28bd80
出典データセット
uspto-grants-1977_07
特許番号
US04036828

関連ノート

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