Isopropylamine → Agn-PC-0nhgeb

HRID 239707

反応式

HRID 239707 の反応式
[CH:1]([NH2:4])([CH3:3])[CH3:2].[CH2:5]1[CH2:11][S:8](=[O:10])(=[O:9])[O:7][CH2:6]1.CCCCCC>ClCCl.CCOCC>[CH:1]([NH:4][CH2:6][CH2:5][CH2:11][S:8]([OH:10])(=[O:9])=[O:7])([CH3:3])[CH3:2]

参加物

5

反応物 3

HCID 6363IsopropylamineHCID 8058HexaneHCID 14264Propane sultone

生成物 1

HCID 11194685Agn-PC-0nhgeb収率 65.8%

試薬・触媒・溶媒 1

HCID 21881112Ethyl ether methylene chloride溶媒

実験手順

Isopropylamine (2.5 mL, 29 mmol) was added to a solution of 1,3-propane sultone (3.05 g, 25 mmol) in a mixture of dichloromethane/ether (40 mL, 1:1). The mixture was heated at reflux for 3 hours. The reaction mixture was cooled to room temperature and hexane (10 mL) was added. The solid material was collected by filtration, rinsed with ether (10 mL), and dried in vacuo. Compound CG was obtained as a fine white powder (2.98 g, 65.6% yield). m.p. 240-43° C. 1H NMR (500 MHz, D2O) δ 1.06 (d, J=6.3 Hz, 6H), 1.86 (qt, J=7.6 Hz, 2H), 2.76 (t, J=7.6 Hz, 2H), 3.14 (t, J=7.8 Hz, 2H), 3.13-3.21 (m, J=6.6 Hz, 1H). 13C NMR (125 MHz, D2O) δ 18.2, 21.5, 25.8, 43.4, 47.9, 50.8.

後処理

  1. temperatureThe mixture was heated
  2. temperatureat reflux for 3 hours
  3. filtrationThe solid material was collected by filtration
  4. washrinsed with ether (10 mL)
  5. customdried in vacuo

出典と根拠

ORDレコード
ord-f8b601054a0045a381270128927e6333
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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