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Tert-butyl[4-(5-methyl-1,3,4-oxadiazol-2-yl)pyridin-2-yl]carbamate → 4-(5-Methyl-1,3,4-oxadiazol-2-yl)pyridin-2-amine

HRID 452625
ノート
印刷プレビュー

反応式

HRID 452625 の反応式
C(OC(=O)[NH:7][C:8]1[CH:13]=[C:12]([C:14]2[O:15][C:16]([CH3:19])=[N:17][N:18]=2)[CH:11]=[CH:10][N:9]=1)(C)(C)C>FC(F)(F)C(O)=O>[CH3:19][C:16]1[O:15][C:14]([C:12]2[CH:11]=[CH:10][N:9]=[C:8]([NH2:7])[CH:13]=2)=[N:18][N:17]=1
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 1

HCID 86640028Tert-butyl[4-(5-methyl-1,3,4-oxadiazol-2-yl)pyridin-2-yl]carbamate

生成物 1

HCID 686630234-(5-Methyl-1,3,4-oxadiazol-2-yl)pyridin-2-amine収率 92%

試薬・触媒・溶媒 1

HCID 6422Trifluoroacetic acid溶媒

実験手順

A mixture of tert-butyl[4-(5-methyl-1,3,4-oxadiazol-2-yl)pyridin-2-yl]carbamate (440 mg, 1.59 mmol) and trifluoroacetic acid (10 mL) was stirred at room temperature for 1.5 hr. The reaction mixture was concentrated under reduced pressure, and the residue was neutralized with saturated aqueous sodium hydrogen carbonate solution, and extracted with ethyl acetate/tetrahydrofuran. The organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate and concentrated under reduced pressure to give the title compound (257 mg, yield 92%) as pale-yellow crystals.

後処理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. extractionextracted with ethyl acetate/tetrahydrofuran
  3. washThe organic layer was washed with saturated brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-a68e55e8e25c46db99f0ec70c13cfffc
出典データセット
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08492378B2

反応ノート

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