Diethyl Ether → HCID 14424276, 화합물

HRID 414222노트

반응식

HRID 414222 반응식
[Br:1][CH2:2][C:3]([C:5]1[S:6][C:7]([CH3:10])=[CH:8][CH:9]=1)=[O:4].[CH2:11]1[N:16]2[CH2:17][N:18]3[CH2:20][N:14]([CH2:15]2)[CH2:13][N:12]1[CH2:19]3.C(OCC)C>C(Cl)(Cl)Cl.C(Cl)Cl>[Br-:1].[O:4]=[C:3]([C:5]1[S:6][C:7]([CH3:10])=[CH:8][CH:9]=1)[CH2:2][N+:12]12[CH2:13][N:14]3[CH2:20][N:18]([CH2:17][N:16]([CH2:15]3)[CH2:11]1)[CH2:19]2

참가 물질

6

반응물 3

HCID 3283Diethyl EtherHCID 4101HexamethylenetetramineHCID 122897372-Bromo-1-(5-methyl-2-thienyl)ethanone

생성물 1

HCID 14424276HCID 14424276, 화합물

시약·촉매·용매 2

HCID 6212Chloroform용매HCID 6344Dichloromethane용매

실험 절차

A mixture of 2-bromo-1-(5-methylthien-2-yl)ethanone (30.0 g of the aforesaid dark liquid) and hexamethylene tetramine (21.0 g, 0.15 mole) in chloroform (500 ml) was stirred at room temperature for three days. The solvent was removed from the reaction mixture by evaporation under reduced pressure, leaving a dark residue. This residue was stirred in warm methylene chloride. Diethyl ether was added slowly to the mixture, causing a solid to precipitate. After being cooled for several hours, the solid was collected by filtration. The filter cake was rinsed with diethyl ether and was dried under reduced pressure yielding 43.1 g of 1-[2-oxo-2-(5-methylthienyl)ethyl]-3,5,7-triaza-1-azoniatricyclo-[3,3,1,13,7 ]decane bromide (mp 141° C. dec).

후처리

  1. customThe solvent was removed from the reaction mixture by evaporation under reduced pressure
  2. customleaving a dark residue
  3. customto precipitate
  4. temperatureAfter being cooled for several hours
  5. filtrationthe solid was collected by filtration
  6. washThe filter cake was rinsed with diethyl ether
  7. customwas dried under reduced pressure

출처 및 근거

ORD 기록
ord-51558efb2e724ccc8c8f6c59ae0ef28c
출처 데이터셋
uspto-grants-1988_12
특허 번호
US04791124

반응 노트

불러오는 중…