Methanol → methyl (2S,4R)-4-(9H-fluoren-9-ylmethoxycarbonylamino)-pyrrolidine-2-carboxylate sulphate

HRID 1641356Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1641356
[CH:1]1[C:13]2[CH:12]([CH2:14][O:15][C:16]([NH:18][C@H:19]3[CH2:23][N:22](C(OC(C)(C)C)=O)[C@H:21]([C:31]([O-:33])=[O:32])[CH2:20]3)=[O:17])[C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]=2[CH:4]=[CH:3][CH:2]=1.[S:34](=[O:38])(=[O:37])([OH:36])[OH:35].[CH3:39]O>>[S:34]([OH:38])([OH:37])(=[O:36])=[O:35].[CH:5]1[C:13]2[CH:12]([CH2:14][O:15][C:16]([NH:18][C@H:19]3[CH2:23][NH:22][C@H:21]([C:31]([O:33][CH3:39])=[O:32])[CH2:20]3)=[O:17])[C:11]3[C:10](=[CH:9][CH:8]=[CH:7][CH:6]=3)[C:1]=2[CH:2]=[CH:3][CH:4]=1

Komponenten

4

Edukt 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 258060671,2-Pyrrolidinedicarboxylic acid, 4-[[(9H-fluoren-9-ylmethoxy)carbonyl]amino]-, 1-(1,1-dimethylethyl) ester, (2S,4R)-

Produkt 1

HCID 66736107methyl (2S,4R)-4-(9H-fluoren-9-ylmethoxycarbonylamino)-pyrrolidine-2-carboxylate sulphate

Versuchsvorschrift

850 mg 1-tert.butyl (2S,4R)-4-(9H-fluoren-9-ylmethoxycarbonylamino)-pyrrolidine-1,2-dicarboxylate and 60 μl sulphuric acid are placed in 12 ml abs. methanol. The reaction mixture is then refluxed for 48 hours with stirring and then evaporated to dryness. 1.0 g product is obtained as a foam. Analytical HPLC-MS (method B): RT=1.80 min.

Aufarbeitung

  1. temperatureThe reaction mixture is then refluxed for 48 hours
  2. customevaporated to dryness

Quellen und Nachweise

ORD-Eintrag
ord-9531a8d7e8e1488685e5f5a29b8ad645
Quelldatensatz
uspto-grants-2012_02
Patentnummer
US08114878B2

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