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1,4-Dioxane hydrochloride → N,N-dibenzylpiperidine-4-carboxamide

HRID 1743816
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HRID 1743816 반응식
[CH2:1]([N:8]([CH2:24][C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1)[C:9]([CH:11]1[CH2:16][CH2:15][N:14](C(OC(C)(C)C)=O)[CH2:13][CH2:12]1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.O1CCOCC1.Cl>CO>[CH2:24]([N:8]([CH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1)[C:9]([CH:11]1[CH2:12][CH2:13][NH:14][CH2:15][CH2:16]1)=[O:10])[C:25]1[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=1
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참가 물질

4

반응물 2

HCID 204431481,4-Dioxane hydrochlorideHCID 22236495Tert-butyl 4-[(dibenzylamino)carbonyl]piperidine-1-carboxylate

생성물 1

HCID 22236499N,N-dibenzylpiperidine-4-carboxamide수율 99%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a stirred solution of tert-butyl 4-[(dibenzylamino)carbonyl]piperidine-1-carboxylate (EXAMPLE 4, Step 1, 4.0 g, 10.0 mmol) in methanol (550 mL) was added 4N HCl dioxane solution (80 mL, 320 mmol) at 0° C. The mixture was stirred for 6 h and evaporated. The resulting amorphous was dissolved in aqueous ammonia and the mixture was extracted with dichloromethane. The combined extract was dried over magnesium sulfate, and concentrated to afford 3.0 g (99%) of the title compound as a colorless amorphous powder.

후처리

  1. customevaporated
  2. dissolutionThe resulting amorphous was dissolved in aqueous ammonia
  3. extractionthe mixture was extracted with dichloromethane
  4. extractionThe combined extract
  5. dry with materialwas dried over magnesium sulfate
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-8b4e349b459b4bc1a86c9757865e9ad7
출처 데이터셋
uspto-grants-2006_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07012080B2

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