Acetonitrile → HCID 58724657、化合物

HRID 239791

反応式

HRID 239791 の反応式
[CH:1]12[CH2:10][CH:5]3[CH2:6][CH:7]([CH2:9][CH:3]([CH2:4]3)[CH:2]1N)[CH2:8]2.[CH3:12][CH:13]1[S:17](=[O:19])(=[O:18])[O:16][CH2:15][CH2:14]1.C(#[N:22])C>>[C:1]12([NH:22][CH2:15][CH2:14][CH:13]([S:17]([OH:16])(=[O:19])=[O:18])[CH3:12])[CH2:10][CH:5]3[CH2:6][CH:7]([CH2:9][CH:3]([CH2:4]3)[CH2:2]1)[CH2:8]2

参加物

4

反応物 3

HCID 6342AcetonitrileHCID 253322-AminoadamantaneHCID 707161,2-Oxathiolane, 3-methyl-, 2,2-dioxide

生成物 1

HCID 58724657HCID 58724657、化合物

実験手順

To a solution of 2-adamantanamine (1.99 g, 13.1 mmol) in acetonitrile (15 mL) was added 2,4-butane sultone (1.87 g, 13.8 mmol). The solution was stirred at reflux for 2 hours. The reaction was cooled to room temperature. The solid was collected by filtration, washed with acetonitrile (3×25 mL) and dried in vacuo. 1H NMR (DMSO, 500 MHz) δ ppm 8.53 (s (broad), 1H), 3.33 (m, 2H), 2.61 (m, 1H), 2.10 (s, 3H), 1.93 (m, 1H), 1.77 (m, 7H), 1.61 (m, 6H), 1.12 (d, 1H, J=6.8 Hz). 13C (DMSO, 125 MHz) δ ppm 56.20, 53.34, 35.85, 29.75, 29.04, 17.206. ES-MS 288 (M+1).

後処理

  1. temperatureat reflux for 2 hours
  2. filtrationThe solid was collected by filtration
  3. washwashed with acetonitrile (3×25 mL)
  4. customdried in vacuo

出典と根拠

ORDレコード
ord-7086b499dd4845fea68036c73b77a6d6
出典データセット
uspto-grants-2014_02
特許番号
US08642801B2

関連ノート

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