Trifluoroacetic acid → 2-(Piperidin-4-yloxy)isoindoline-1,3-dione trifluoroacetic acid

HRID 1895898ノート

反応式

HRID 1895898 の反応式
[O:1]=[C:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:4](=[O:11])[N:3]1[O:12][CH:13]1[CH2:18][CH2:17][N:16](C(OC(C)(C)C)=O)[CH2:15][CH2:14]1.[F:26][C:27]([F:32])([F:31])[C:28]([OH:30])=[O:29]>>[F:26][C:27]([F:32])([F:31])[C:28]([OH:30])=[O:29].[NH:16]1[CH2:17][CH2:18][CH:13]([O:12][N:3]2[C:2](=[O:1])[C:10]3[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=3)[C:4]2=[O:11])[CH2:14][CH2:15]1

参加物

3

反応物 2

HCID 6422Trifluoroacetic acidHCID 21751544Tert-butyl 4-(1,3-dioxoisoindolin-2-yloxy)piperidine-1-carboxylate

生成物 1

HCID 671183852-(Piperidin-4-yloxy)isoindoline-1,3-dione trifluoroacetic acid収率 90%

実験手順

tert-Butyl 4-(1,3-dioxoisoindolin-2-yloxy)piperidine-1-carboxylate (3.81 g, 11.0 mmol) was added to trifluoroacetic acid (80 ml) and the mixture was stirred at room temperature for 30 minutes. The reaction was concentrated in vacuo and the residue was triturated with diethyl ether (100 ml). The resulting solid was washed with diethyl ether (20 ml×3) to give 2-(piperidin-4-yloxy)isoindoline-1,3-dione trifluoroacetic acid (3.50 g, 90%) as a white solid: LCMS: 247 [M+1]+.

後処理

  1. concentrationThe reaction was concentrated in vacuo
  2. customthe residue was triturated with diethyl ether (100 ml)
  3. washThe resulting solid was washed with diethyl ether (20 ml×3)

出典と根拠

ORDレコード
ord-168fafd5c86d428fb1c805279023fa9a
出典データセット
uspto-grants-2013_08
特許番号
US08518934B2

反応ノート

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