Hydrochloric Acid → Methyl 6-aminoquinoline-3-carboxylate dihydrochloride

HRID 1894957ノート

反応式

HRID 1894957 の反応式
C(OC([NH:8][C:9]1[CH:10]=[C:11]2[C:16](=[CH:17][CH:18]=1)[N:15]=[CH:14][C:13]([C:19]([O:21][CH3:22])=[O:20])=[CH:12]2)=O)(C)(C)C.[ClH:23].O1CCOCC1>C(Cl)Cl>[ClH:23].[ClH:23].[NH2:8][C:9]1[CH:10]=[C:11]2[C:16](=[CH:17][CH:18]=1)[N:15]=[CH:14][C:13]([C:19]([O:21][CH3:22])=[O:20])=[CH:12]2

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 67002181Methyl 6-(tert-butoxycarbonylamino)quinoline-3-carboxylate

生成物 1

HCID 67002244Methyl 6-aminoquinoline-3-carboxylate dihydrochloride

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of methyl 6-[(tert-butoxycarbonyl)amino]quinoline-3-carboxylate (Int-2, 1.28 g, 4.23 mmol) in methylene chloride (38 mL) was added hydrochloric acid in 1,4-dioxane (4.0 M, 10.6 mL, 42.3 mmol). The reaction was stirred at room temperature overnight then concentrated under reduced pressure. The crude reside was dried in vacuo and used as obtained. LC-MS: (FA) ES+ 203; 1H NMR (400 MHz, d6-DMSO) δ ppm 9.14 (s, 1H), 9.08 (d, J=1.8 Hz, 1H), 8.10 (d, J=9.1 Hz, 1H), 7.62 (dd, J=9.1, 2.4 Hz, 1H), 7.33 (d, J=1.7 Hz, 1H), 3.96 (s, 9H).

後処理

  1. concentrationthen concentrated under reduced pressure
  2. customThe crude reside was dried in vacuo
  3. customas obtained

出典と根拠

ORDレコード
ord-1d17512a48954b0083454f4a875fba2c
出典データセット
uspto-grants-2013_08
特許番号
US08513421B2

反応ノート

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