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

HRID 634957
ノート
印刷プレビュー

反応式

HRID 634957 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 2

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

生成物 1

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

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-551bfe40c7de47a080ca8d466a9656aa
出典データセット
uspto-grants-2001_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06184382B2

反応ノート

読み込み中…

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