Hydrochloric Acid → 4-Piperidin-1-yl-but-2-enoic acid-HCl

HRID 467604ノート

反応式

HRID 467604 の反応式
C[O:2][C:3](=[O:13])[CH:4]=[CH:5][CH2:6][N:7]1[CH2:12][CH2:11][CH2:10][CH2:9][CH2:8]1.[ClH:14]>>[ClH:14].[N:7]1([CH2:6][CH:5]=[CH:4][C:3]([OH:13])=[O:2])[CH2:12][CH2:11][CH2:10][CH2:9][CH2:8]1

参加物

3

反応物 2

HCID 313Hydrochloric AcidHCID 572293064-Piperidin-1-yl-but-2-enoic acid methyl ester

生成物 1

HCID 698441674-Piperidin-1-yl-but-2-enoic acid-HCl収率 17%

実験手順

4-Piperidin-1-yl-but-2-enoic acid methyl ester (2.05 g, 11.2 mmol) and concentrated hydrochloric acid (10 mL) were combined in dioxanes (30 mL) and heated to reflux overnight. The mixture was concentrated in vacuo. The residue was crystallized from IPA to yield the desired product (390 mg, 17%). 400 MHz 1H NMR (DMSO-d6) δ 6.80 (dt, 1H, J=15.6, 7.1 Hz), 6.14 (d, 1H, J=15.6 Hz), 3.85 (d, 1H, J=7.1 Hz), 2.89 (m, 4H), 1.54 (m, 6H). MS m/z 170 (M+1).

後処理

  1. temperatureheated
  2. temperatureto reflux overnight
  3. concentrationThe mixture was concentrated in vacuo
  4. customThe residue was crystallized from IPA

出典と根拠

ORDレコード
ord-04ac8d251b934e5ebf7ed767bda7eb9f
出典データセット
uspto-grants-2014_01
特許番号
US08623883B2

反応ノート

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