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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Triethylamine → cis(+/-)-3-(tert-Butoxycarbonyl)amino-1-(diphenylmethyl)-2-ethylazetidine

HRID 43920
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HRID 43920 반응식
[C:1](OC([O-])=O)([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])=[O:2].C(N(CC)CC)C.[C:19]1([CH:25]([C:33]2[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=2)[N:26]2[CH2:29][C@H:28]([NH2:30])[C@@H:27]2[CH2:31][CH3:32])[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1>ClCCl.C(OCC)(=O)C>[C:4]([O:3][C:1]([NH:30][C@H:28]1[CH2:29][N:26]([CH:25]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[C:33]2[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=2)[C@H:27]1[CH2:31][CH3:32])=[O:2])([CH3:7])([CH3:6])[CH3:5]
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참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 10038572cis(+/-)-1-(Diphenylmethyl)-2-ethylazetidin-3-amineHCID 22064466Tert-butyldicarbonate

생성물 1

HCID 86648819cis(+/-)-3-(tert-Butoxycarbonyl)amino-1-(diphenylmethyl)-2-ethylazetidine수율 57.1%

시약·촉매·용매 2

HCID 6344Dichloromethane용매
HCID 8857
Ethyl Acetate
용매

실험 절차

tert-Butyl dicarbonate (202 mg, 0.93 mmol) and triethylamine (0.27 mL, 1.93 mmol) were added to a solution of cis(±)-1-(diphenylmethyl)-2-ethylazetidin-3-amine obtained in Example (235d) (206 mg, 0.77 mmol) in dichloromethane (4 mL), followed by stirring for two hours. The reaction solution was diluted with ethyl acetate, and the organic layer was washed with water and brine. The organic layer was dried over anhydrous magnesium sulfate. Following filtration, the filtrate was concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (elution solvent: hexane/ethyl acetate=4/1) to obtain 161 mg of the title compound as a colorless oily substance (57%).

후처리

  1. washthe organic layer was washed with water and brine
  2. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  3. filtrationfiltration
  4. concentrationthe filtrate was concentrated under reduced pressure
  5. customThe resulting residue was purified by silica gel column chromatography (elution solvent: hexane/ethyl acetate=4/1)

출처 및 근거

ORD 기록
ord-67eecd99761e4b2093029e1d13093321
출처 데이터셋
uspto-grants-2013_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08536197B2

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