3-Azaspiro(5.5)undecane hydrochloride → HCID 68619688、化合物

HRID 1042242

反応式

HRID 1042242 の反応式
[CH2:1]1[C:6]2([CH2:11][CH2:10][CH2:9][CH2:8][CH2:7]2)[CH2:5][CH2:4][NH:3][CH2:2]1.[IH:12].CS[C:15]1[NH:16][CH2:17][CH2:18][N:19]=1>CO>[IH:12].[NH:19]1[CH2:18][CH2:17][N:16]=[C:15]1[N:3]1[CH2:4][CH2:5][C:6]2([CH2:11][CH2:10][CH2:9][CH2:8][CH2:7]2)[CH2:1][CH2:2]1

参加物

4

反応物 2

HCID 4174123-Azaspiro(5.5)undecane hydrochlorideHCID 122212281H-Imidazole, 4,5-dihydro-2-(methylthio)-, hydriodide (1:1)

生成物 1

HCID 68619688HCID 68619688、化合物収率 65%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

3-Azaspiro[5,5]undecane (0.38 g, 2 mmol) and 2-methylthio-2-imidazoline hydroiodide (0.44 g, 1.8 mmol) was refluxing in CH3OH overnight, concentrated in vacuo and purified by flash chromatography to give yellow oil (0.26 g, 65% yield). 1H NMR (360 MHz, CDCl3) δ 8.27 (br s, 2H), 3.72 (s, 4H), 3.39 (t, J=5.83 Hz, 4H), 1.50 (t, J=5.94 Hz, 4H), 1.47-1.44 (m, 10H); 13C NMR (90 MHz, CDCl3) δ 159.48, 43.39, 42.73, 36.02, 35.26, 30.83, 26.65, 21.61. 21.49; ESI-MS: Calculated for C13H24IN3 (M−I)+ 222.3, Found: 222.5.

後処理

  1. concentrationconcentrated in vacuo
  2. custompurified by flash chromatography

出典と根拠

ORDレコード
ord-3e292b52922e4f0f8ce663087f604858
出典データセット
uspto-grants-2013_10
特許番号
US08557836B2

関連ノート

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