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Trifluoroacetic acid → 6-Methoxyquinolin-3-amine

HRID 495471
ノート
印刷プレビュー

反応式

HRID 495471 の反応式
C(OC([N:8]1[C:17]2[C:12](=[CH:13][C:14]([O:18][CH3:19])=[CH:15][CH:16]=2)[CH:11]=[C:10]([NH2:20])[CH2:9]1)=O)(C)(C)C.C(O)(C(F)(F)F)=O>C(Cl)Cl>[CH3:19][O:18][C:14]1[CH:13]=[C:12]2[C:17](=[CH:16][CH:15]=1)[N:8]=[CH:9][C:10]([NH2:20])=[CH:11]2
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 22326880N-tert-butyloxycarbonyl-6-methoxy-3-aminoquinoline

生成物 1

HCID 5999396-Methoxyquinolin-3-amine

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a stirred solution of N-tert-butyloxycarbonyl-6-methoxy-3-aminoquinoline (Step F, 3 g, 0.011 mol) in CH2Cl2 (50 mL) cooled at 0° C. was added TFA (8.4 mL, 0.11 mL). The reaction mixture was warmed to RT and stirred for 8 h. The reaction mixture was concentrated under vacuum. The residue was suspended into MTBE. The yellow solid was filtered off and washed with MTBE. The dry yellow solid was suspended in NaOH 1N and the suspension was stirred for 15 min. The resulting slurry was filtered. The solid was washed with water and dried over P2O5 to give 6-methoxy-3-aminoquinoline as a white solid.

後処理

  1. concentrationThe reaction mixture was concentrated under vacuum
  2. filtrationThe yellow solid was filtered off
  3. washwashed with MTBE
  4. stirringthe suspension was stirred for 15 min
  5. filtrationThe resulting slurry was filtered
  6. washThe solid was washed with water
  7. dry with materialdried over P2O5

出典と根拠

ORDレコード
ord-2ae50e70428f4a12879f6b940baedac9
出典データセット
uspto-grants-2005_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06939874B2

反応ノート

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