1-Amino-2-propanol → 2,8-Dimethyl-1-oxa-4,8-diazaspiro[4.5]decane

HRID 1187318

反応式

HRID 1187318 の反応式
[NH2:1][CH2:2][CH:3]([OH:5])[CH3:4].[CH3:6][N:7]1[CH2:12][CH2:11][C:10](=O)[CH2:9][CH2:8]1>>[CH3:4][CH:3]1[CH2:2][NH:1][C:10]2([CH2:11][CH2:12][N:7]([CH3:6])[CH2:8][CH2:9]2)[O:5]1

参加物

3

反応物 2

HCID 41-Amino-2-propanolHCID 740491-Methyl-4-piperidone

生成物 1

HCID 220974902,8-Dimethyl-1-oxa-4,8-diazaspiro[4.5]decane

実験手順

A mixture of 1-amino-2-propanol (9.2 ml, 1.2 mmol) and 1-methyl-4-piperidone (11.5 ml, 1.0 mmol) was heated under reflux for 2 h and left overnight at room temperature. The reaction mixture was distilled under reduced pressure (˜15 mm Hg). The title compound was collected at 82-95° C. 1H NMR (CDCl3, 300 MHz) δ 4.02 (m, 1H, OCH), 3.25 (dd, J=11.9, 6.3 Hz, 1H, CHH), 2.68 (dd, J=11.9, 6.6 Hz, 1H, CHH), 2.4-2.6 (m, 4H-piperidine), 2.1 (s, 3H, NCH3), 1.65-1.81 (m, 4H-piperidine), 1.21 (d, J=6.1 Hz, 3H, CH3CH) ppm.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 2 h
  3. distillationThe reaction mixture was distilled under reduced pressure (˜15 mm Hg)
  4. customThe title compound was collected at 82-95° C

出典と根拠

ORDレコード
ord-83e39f763e7240b58d20ae3a9e3ac0db
出典データセット
uspto-grants-2014_03
特許番号
US08673931B2

関連ノート

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