1,2-Dimethylpropylamine → 1-Propanesulfonic acid, 3-[(1,2-dimethylpropyl)amino]-

HRID 239743

反応式

HRID 239743 の反応式
[CH3:1][CH:2]([NH2:6])[CH:3]([CH3:5])[CH3:4].[CH2:7]1[CH2:13][S:10](=[O:12])(=[O:11])[O:9][CH2:8]1>O1CCCC1>[CH3:1][CH:2]([NH:6][CH2:8][CH2:7][CH2:13][S:10]([OH:12])(=[O:11])=[O:9])[CH:3]([CH3:5])[CH3:4]

参加物

4

反応物 2

HCID 117311,2-DimethylpropylamineHCID 14264Propane sultone

生成物 1

HCID 114812161-Propanesulfonic acid, 3-[(1,2-dimethylpropyl)amino]-

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a solution of 1,2-dimethylpropylamine (10.0 g, 115 mmol) in tetrahydrofuran (80 mL) was slowly added a solution of 1,3-propane sultone (13.7 g, 110 mmol) in THF (20 mL). The solution was stirred at reflux for 2 hours. The reaction mixture was cooled to room temperature. The solid product was collected by filtration, washed with THF (50 mL) and EtOH (50 mL). The resulting solid was dried in vacuo, to afford compound DQ (17.5 g, 76%). 1H NMR (D2O, 500 MHz) δ ppm 3.07 (m, 3H), 2.88 (t, 2H, J=7.3 Hz), 1.97 (m, 3H), 1.10 (d, 3H, J=6.8 Hz), 0.85 (d, 3H, J=6.8 Hz), 0.81 (d, 3H, J=6.8 Hz). 13C NMR (D2O, 125 MHz) δ ppm 59.79, 48.19, 44.18, 29.72, 21.51, 18.44, 15.02, 10.71. ES-MS 232 (M+Na).

後処理

  1. temperatureat reflux for 2 hours
  2. filtrationThe solid product was collected by filtration
  3. washwashed with THF (50 mL) and EtOH (50 mL)
  4. customThe resulting solid was dried in vacuo
  5. customto afford compound DQ (17.5 g, 76%)

出典と根拠

ORDレコード
ord-af6c9691b0c443de8ca4aaaef90cde59
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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