Diethyl Ether → HCID 14424276、化合物

HRID 414222ノート

反応式

HRID 414222 の反応式
[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

参加物

6

反応物 3

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

生成物 1

HCID 14424276HCID 14424276、化合物

試薬・触媒・溶媒 2

HCID 6212Chloroform溶媒HCID 6344Dichloromethane溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-51558efb2e724ccc8c8f6c59ae0ef28c
出典データセット
uspto-grants-1988_12
特許番号
US04791124

反応ノート

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