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4-Methylmorpholine → 2-[3,3-Bis(tert-butoxycarbonylamino)-2-oxo-piperidin-1-yl]-propionic acid ethyl ester

HRID 2039001
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HRID 2039001 반응식
CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.[C:25]([O:29][C:30]([NH:32][C:33]([NH:48][C:49]([O:51][C:52]([CH3:55])([CH3:54])[CH3:53])=[O:50])([CH2:37][CH2:38][CH2:39][NH:40][CH:41]([C:43]([O:45][CH2:46][CH3:47])=[O:44])[CH3:42])[C:34]([OH:36])=O)=[O:31])([CH3:28])([CH3:27])[CH3:26].CN1CCOCC1>CN(C)C=O>[CH2:46]([O:45][C:43](=[O:44])[CH:41]([N:40]1[CH2:39][CH2:38][CH2:37][C:33]([NH:48][C:49]([O:51][C:52]([CH3:55])([CH3:53])[CH3:54])=[O:50])([NH:32][C:30]([O:29][C:25]([CH3:27])([CH3:26])[CH3:28])=[O:31])[C:34]1=[O:36])[CH3:42])[CH3:47]
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참가 물질

5

반응물 3

HCID 79724-MethylmorpholineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 866488792,2-Bis(tert-butoxycarbonylamino)-5-(1-ethoxycarbonyl-ethylamino)-pentanoic acid

생성물 1

HCID 866488782-[3,3-Bis(tert-butoxycarbonylamino)-2-oxo-piperidin-1-yl]-propionic acid ethyl ester수율 86.7%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

HATU (1.72 g, 4.5 mmol) was added to a solution of 2,2-bis(tert-butoxycarbonylamino)-5-(1-ethoxycarbonyl-ethylamino)-pentanoic acid (1.31 g, 3.0 mmol) and 4-methylmorpholine in dimethylformamide (50 mL). After 30 minutes the solvent was removed under reduced pressure and the residue was subjected to flash chromatography with eluent of ethyl acetate and hexane. The product-containing fractions were combined and the solvent was removed under reduced pressure to provide 2-[3,3-bis(tert-butoxycarbonylamino)-2-oxo-piperidin-1-yl]-propionic acid ethyl ester (1.11 g, 2.6 mmol, 86%). C20H34N2O7 calculated 414.2 observed [M+1]+ 415.2; rt=2.77 min.

후처리

  1. customAfter 30 minutes the solvent was removed under reduced pressure
  2. customthe solvent was removed under reduced pressure

출처 및 근거

ORD 기록
ord-be1f85d5d8dd4745a2dff11531699c58
출처 데이터셋
uspto-grants-2013_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08575118B2

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