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

HRID 634957
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HRID 634957 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

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

생성물 1

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

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-551bfe40c7de47a080ca8d466a9656aa
출처 데이터셋
uspto-grants-2001_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06184382B2

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