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

HRID 1258443ノート

反応式

HRID 1258443 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-c8a6885ab1e54b8b9cf0ea3e834c4ee2
出典データセット
uspto-grants-2013_06
特許番号
US08466165B2

反応ノート

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