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Hydrogen chloride-ethyl acetate → phenylmethyl 1-[N-(piperazine-1-carbonyl)amino]cyclohexanecarboxylate

HRID 1953432
ノート
印刷プレビュー

反応式

HRID 1953432 の反応式
CC(OC([N:8]1[CH2:13][CH2:12][N:11]([C:14]([NH:16][C:17]2([C:23]([O:25][CH2:26][C:27]3[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=3)=[O:24])[CH2:22][CH2:21][CH2:20][CH2:19][CH2:18]2)=[O:15])[CH2:10][CH2:9]1)=O)(C)C.Cl.C(OCC)(=O)C>C(OCC)(=O)C.Cl>[N:11]1([C:14]([NH:16][C:17]2([C:23]([O:25][CH2:26][C:27]3[CH:28]=[CH:29][CH:30]=[CH:31][CH:32]=3)=[O:24])[CH2:22][CH2:21][CH2:20][CH2:19][CH2:18]2)=[O:15])[CH2:12][CH2:13][NH:8][CH2:9][CH2:10]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 21866389Hydrogen chloride-ethyl acetateHCID 53984920phenylmethyl 1-[N-[4-(2-methyl-2-propyloxycarbonyl)piperazine-1-carbonyl]amino]cyclohexanecarboxylate

生成物 1

HCID 23297891phenylmethyl 1-[N-(piperazine-1-carbonyl)amino]cyclohexanecarboxylate収率 87.9%

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 8857Ethyl Acetate
溶媒

実験手順

2.5 g (5.6 mmol) of phenylmethyl 1-[N-[4-(2-methyl-2-propyloxycarbonyl) piperazine-1-carbonyl]amino]cyclohexanecarboxylate synthesized in Reference Example 8 was dissolved in ethyl acetate and 14 ml (56 mmol) of 4N hydrogenchloride-ethyl acetate solution (56 mmol) was added to the above prepared mixture under 0° C. and stirred for 3 hours at the room temperature. After completion of concentration of the reaction solution, the reaction solution was dissolved in 1N hydrochloric acid and washed with ethyl acetate. The water layer was separated out and was made into pH 9 with the addition of sodium carbonate and extracted three times with chloroform. The chloroform layer was dried over anhydrous sodium sulfate and concentrated under reduced pressure, whereby 1.7 g of phenylmethyl 1-[N-(piperazine-1-carbonyl)amino]cyclohexanecarboxylate was obtained.

後処理

  1. washwashed with ethyl acetate
  2. customThe water layer was separated out
  3. additionwas made into pH 9 with the addition of sodium carbonate
  4. extractionextracted three times with chloroform
  5. dry with materialThe chloroform layer was dried over anhydrous sodium sulfate
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-2ecc96b7780e4d0998e17af5ce964204
出典データセット
uspto-grants-2000_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06117870

反応ノート

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