Octylamine → 4-(Octylamino)butane-2-sulfonic acid

HRID 239790

反応式

HRID 239790 の反応式
[CH2:1]([NH2:9])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH3:8].[CH3:10][CH:11]1[S:15](=[O:17])(=[O:16])[O:14][CH2:13][CH2:12]1>CC(=O)CC>[CH2:1]([NH:9][CH2:13][CH2:12][CH:11]([S:15]([OH:17])(=[O:16])=[O:14])[CH3:10])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH3:8]

参加物

4

反応物 2

HCID 8143OctylamineHCID 707161,2-Oxathiolane, 3-methyl-, 2,2-dioxide

生成物 1

HCID 589318174-(Octylamino)butane-2-sulfonic acid

試薬・触媒・溶媒 1

HCID 6569Methyl Ethyl Ketone溶媒

実験手順

To a solution of octylamine (2.00 g, 15.5 mmol) in 2-butanone (17 mL) was added 2,4-butane sultone (2.21 g, 16.2 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 acetone (2×25 mL) and dried in vacuo. It was suspended in a solution of 25% EtOH/acetone (50 mL). The suspension was stirred for 5 minutes. The solid was collected by filtration, washed with acetone (2×25 mL) and dried in vacuo. 1H NMR (DMSO, 500 MHz) δ ppm 8.45 (s (broad), 1H), 3.01 (m, 1H), 2.84 (m, 2H), 2.58 (m, 1H), 1.92 (m, 1H), 1.75 (m, 1H), 1.51 (m, 2H), 1.10 (d, 1H, J=6.8 Hz), 0.85 (t, 3H, J=6.8 Hz). 13C (DMSO, 125 MHz) δ ppm 53.05, 47.27, 46.15, 31.83, 29.42, 29.13, 26.51, 26.27, 22.75, 17.19, 14.64. ES-MS 266 (M+1).

後処理

  1. temperatureat reflux for 2 hours
  2. filtrationThe solid was collected by filtration
  3. washwashed with acetone (2×25 mL)
  4. customdried in vacuo
  5. stirringThe suspension was stirred for 5 minutes
  6. filtrationThe solid was collected by filtration
  7. washwashed with acetone (2×25 mL)
  8. customdried in vacuo

出典と根拠

ORDレコード
ord-6e42ac5af2254733960c987094f5368b
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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