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Trifluoroacetic acid → 4-(5-Piperidin-4-yl-1,2,4-oxadiazol-3-yl)pyridine

HRID 221357
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反応式

HRID 221357 の反応式
FC(F)(F)C(O)=O.C(OC([N:15]1[CH2:20][CH2:19][CH:18]([C:21]2[O:25][N:24]=[C:23]([C:26]3[CH:31]=[CH:30][N:29]=[CH:28][CH:27]=3)[N:22]=2)[CH2:17][CH2:16]1)=O)(C)(C)C>C(Cl)Cl>[NH:15]1[CH2:20][CH2:19][CH:18]([C:21]2[O:25][N:24]=[C:23]([C:26]3[CH:31]=[CH:30][N:29]=[CH:28][CH:27]=3)[N:22]=2)[CH2:17][CH2:16]1
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 57954381HCID 57954381、化合物

生成物 1

HCID 27611434-(5-Piperidin-4-yl-1,2,4-oxadiazol-3-yl)pyridine

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Trifluoroacetic acid (20 ml) was added to a stirred solution of 4-(3-pyridin-4-yl-[1,2,4]oxadiazol-5-yl)piperidine-1-carboxylic acid tert-butyl ester (Example 2, 1.64 g, 4.96 mmol) in CH2Cl2 (35 ml). After 2.5 h at rt, the solvent was evaporated under reduced pressure. The residual solid was suspended in EtOAc (150 ml) and washed with saturated aqueous Na2CO3 (20 ml). The aqueous was separated and extracted with EtOAc (3×30 ml). The combined organic extracts were dried (MgSO4) and evaporated under reduced pressure to afford the title compound: RT=3.48 min, m/z (ES+)=231.2 [M+H]+.

後処理

  1. customthe solvent was evaporated under reduced pressure
  2. washwashed with saturated aqueous Na2CO3 (20 ml)
  3. customThe aqueous was separated
  4. extractionextracted with EtOAc (3×30 ml)
  5. dry with materialThe combined organic extracts were dried (MgSO4)
  6. customevaporated under reduced pressure

出典と根拠

ORDレコード
ord-19e6641f26994c159f56e6339993d2d0
出典データセット
uspto-grants-2012_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08207147B2

反応ノート

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