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Hydrochloric Acid → 2-([1,2,4]Triazolo[4,3-a]pyridin-3-yl)-8-(3,3-difluoropiperidin-4-yloxy)-6-fluoroquinoline dihydrochloride salt

HRID 2035639
ノート
印刷プレビュー

反応式

HRID 2035639 の反応式
[N:1]1[N:2]=[C:3]([C:10]2[CH:19]=[CH:18][C:17]3[C:12](=[C:13]([O:21][CH:22]4[CH2:27][CH2:26][N:25](C(OC(C)(C)C)=O)[CH2:24][C:23]4([F:36])[F:35])[CH:14]=[C:15]([F:20])[CH:16]=3)[N:11]=2)[N:4]2[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=12.[ClH:37].O1CCOCC1.CCOCC>CO>[ClH:37].[ClH:37].[N:1]1[N:2]=[C:3]([C:10]2[CH:19]=[CH:18][C:17]3[C:12](=[C:13]([O:21][CH:22]4[CH2:27][CH2:26][NH:25][CH2:24][C:23]4([F:36])[F:35])[CH:14]=[C:15]([F:20])[CH:16]=3)[N:11]=2)[N:4]2[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=12
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 313Hydrochloric Acid2 回HCID 3283Diethyl EtherHCID 312751,4-DioxaneHCID 67234219Tert-butyl 4-(2-([1,2,4]triazolo[4,3-a]pyridin-3-yl)-6-fluoroquinolin-8-yloxy)-3,3-difluoropiperidine-1-carboxylate

生成物 1

HCID 672344932-([1,2,4]Triazolo[4,3-a]pyridin-3-yl)-8-(3,3-difluoropiperidin-4-yloxy)-6-fluoroquinoline dihydrochloride salt

試薬・触媒・溶媒

1
HCID 887Methanol溶媒

実験手順

tert-Butyl 4-(2-([1,2,4]triazolo[4,3-a]pyridin-3-yl)-6-fluoroquinolin-8-yloxy)-3,3-difluoropiperidine-1-carboxylate (0.072 g, 0.144 mmol) was dissolved in MeOH (0.72 mL) and treated with 4.0 M HCl in dioxane (0.360 mL, 1.44 mmol), then stirred at ambient temperature for 2 hours. The reaction mixture was concentrated in vacuo. The residue was taken up in MeOH and concentrated three times. The residue was chromatographed on SiO2 eluting with a gradient of 2% NH4OH in isopropanol/methylene chloride. The desired product was dissolved in MeOH (2 mL), treated with 2.0 M HCl in ether (0.809 mL, 1.62 mmol) and concentrated in vacuo. The residue was again dissolve in MeOH and concentrated in vacuo several times, then placed under vacuum to give the desired product as a white solid (27.8 mg). MS APCI (+) m/z 400.3 (M+1) detected.

後処理

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. concentrationconcentrated three times
  3. customThe residue was chromatographed on SiO2 eluting with a gradient of 2% NH4OH in isopropanol/methylene chloride
  4. dissolutionThe desired product was dissolved in MeOH (2 mL)
  5. concentrationconcentrated in vacuo
  6. dissolutionThe residue was again dissolve in MeOH
  7. concentrationconcentrated in vacuo several times

出典と根拠

ORDレコード
ord-26433fdccaaf4e429eb70fdd005a0537
出典データセット
uspto-grants-2013_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08575145B2

反応ノート

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