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

HRID 2039001
ノート
印刷プレビュー

反応式

HRID 2039001 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-be1f85d5d8dd4745a2dff11531699c58
出典データセット
uspto-grants-2013_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08575118B2

反応ノート

読み込み中…

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