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N-Ethyl-N-4-piperidinylacetamide → HCID 19761220, 화합물

HRID 249349
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HRID 249349 반응식
[NH:1]1[CH2:6][CH2:5][CH:4]([N:7]([CH2:11][CH3:12])[C:8](=[O:10])[CH3:9])[CH2:3][CH2:2]1.S(C1C=CC(C)=CC=1)(O)(=O)=O.[CH3:24][CH:25]1[C:28]2=[CH:29][CH:30]=[CH:31][CH:32]=[C:27]2[CH2:26]1>C1(C)C=CC=CC=1>[C:25]1([CH2:24][N:1]2[CH2:6][CH2:5][CH:4]([N:7]([CH2:11][CH3:12])[C:8](=[O:10])[CH3:9])[CH2:3][CH2:2]2)[C:28]2[CH:29]=[CH:30][CH:31]=[CH:32][C:27]=2[CH:26]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 19761198N-Ethyl-N-4-piperidinylacetamideHCID 131717785HCID 131717785, 화합물

생성물 1

HCID 19761220HCID 19761220, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

3.3 g of N-piperid-4-yl-N-ethylacetamide and 2.8 g of 1-methylbenzocyclobutene tosylate (prepared in accordance with the process described in J.A.C.S., (1975), 154, p. 347) are refluxed under nitrogen for 20 hours in 16 ml of toluene. After cooling, the reaction mixture is evaporated to dryness and taken up in diethyl ether. After extraction with N hydrochloric acid, the extract is rendered basic in the presence of diethyl ether and the organic phase is washed with water, dried over magnesium sulphate and evaporated in vacuo to yield N-[1-(benzocyclobuten-1-ylmethyl)-piperid-4-yl]-N-ethylacetamide. The corresponding hydrochloride is obtained in ethyl acetate in the presence of ethereal hydrogen chloride.

후처리

  1. temperatureAfter cooling
  2. customthe reaction mixture is evaporated to dryness
  3. extractionAfter extraction with N hydrochloric acid
  4. washthe organic phase is washed with water
  5. dry with materialdried over magnesium sulphate
  6. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-bc3b54992352458888efd1e5926705d8
출처 데이터셋
uspto-grants-1993_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05214055

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