Isopropylamine → Agn-PC-0nhgeb

HRID 239707

반응식

HRID 239707 반응식
[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]

참가 물질

5

반응물 3

HCID 6363IsopropylamineHCID 8058HexaneHCID 14264Propane sultone

생성물 1

HCID 11194685Agn-PC-0nhgeb수율 65.8%

시약·촉매·용매 1

HCID 21881112Ethyl ether methylene chloride용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f8b601054a0045a381270128927e6333
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08642801B2

연결된 노트

불러오는 중…