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Hydrochloric Acid → N-ethyl 2,3-dihydroxycyclopentane carboxamide dihydrochloride hydrate

HRID 634957
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 634957
[ClH:1].[CH2:2]([NH:4][C:5]([CH:7]1[CH2:11][CH2:10][CH:9]([OH:12])[CH:8]1[OH:13])=[O:6])[CH3:3]>>[OH2:6].[ClH:1].[ClH:1].[CH2:2]([NH:4][C:5]([CH:7]1[CH2:11][CH2:10][CH:9]([OH:12])[CH:8]1[OH:13])=[O:6])[CH3:3]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

3

Edukt 2

HCID 313Hydrochloric AcidHCID 23103472N-ethyl-2,3-dihydroxycyclopentanecarboxamide

Produkt 1

HCID 70107347N-ethyl 2,3-dihydroxycyclopentane carboxamide dihydrochloride hydrate

Versuchsvorschrift

The zinc metal and any other insoluble impurities are then removed by filtration of the contents of vessel and the filtrate is collected in another reaction vessel. Acid hydrolysis of [3aR-[3aα,4α,6a(R*),6aα]]-6-[4-[[1-[(3-chlorothien-2-yl)methyl]propyl]amino]-3-aminopyrid-2-ylamino] N-ethyl tetrahydro-2,2-dimethyl-4H-cyclopenta-1,3-dioxole-4-carboxamide (XIII) is then effected by adding concentrated HCl to the second reaction vessel and heating until conversion to [1S-[1α,2β,3β,4α(S*)]]-4-[3-amino-4-[[1-[3-chlorothien-2-yl)methyl]propyl]amino]pyrid-2-ylamino] N-ethyl 2,3-dihydroxycyclopentanecarboxamide (XIII) is essentially complete. Cooling of the second reaction vessel results in crystallization of [1S-[1α,2β,3β,4α(S*)]]-4-[3-amino-4-[[1-[3-chlorothien-2-yl)methyl]propyl]amino]pyrid-2-ylamino] N-ethyl 2,3-dihydroxycyclopentane carboxamide dihydrochloride hydrate which is isolated by filtration.

Aufarbeitung

  1. customThe zinc metal and any other insoluble impurities are then removed by filtration of the contents of vessel
  2. customthe filtrate is collected in another reaction vessel
  3. customAcid hydrolysis of [3aR-[3aα,4α,6a(R*),6aα]]-6-[4-[[1-[(3-chlorothien-2-yl)methyl]propyl]amino]-3-aminopyrid-2-ylamino] N-ethyl tetrahydro-2,2-dimethyl-4H-cyclopenta-1,3-dioxole-4-carboxamide (XIII)
  4. temperatureCooling of the second reaction vessel

Quellen und Nachweise

ORD-Eintrag
ord-551bfe40c7de47a080ca8d466a9656aa
Quelldatensatz
uspto-grants-2001_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06184382B2

Notizen zur Reaktion

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