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

HRID 1953432
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HRID 1953432 반응식
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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매HCID 8857Ethyl Acetate
용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-2ecc96b7780e4d0998e17af5ce964204
출처 데이터셋
uspto-grants-2000_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06117870

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