Hydrochloric Acid → Sepazonium chloride

HRID 1730219ノート

反応式

HRID 1730219 の反応式
Cl.[Br-].[Cl:3][C:4]1[CH:34]=[C:33]([Cl:35])[CH:32]=[CH:31][C:5]=1[CH:6]([O:21][CH2:22][C:23]1[CH:28]=[CH:27][C:26]([Cl:29])=[CH:25][C:24]=1[Cl:30])[CH2:7][N+:8]1[CH:12]=[CH:11][N:10]([CH2:13][CH2:14][C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[CH:9]=1>CO>[Cl-:3].[Cl:3][C:4]1[CH:34]=[C:33]([Cl:35])[CH:32]=[CH:31][C:5]=1[CH:6]([O:21][CH2:22][C:23]1[CH:28]=[CH:27][C:26]([Cl:29])=[CH:25][C:24]=1[Cl:30])[CH2:7][N+:8]1[CH:12]=[CH:11][N:10]([CH2:13][CH2:14][C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[CH:9]=1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 86734178HCID 86734178、化合物

生成物 1

HCID 65336Sepazonium chloride

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

0.2 Mole of gaseous hydrogen chloride is dissolved in 32 parts of methanol and to this solution are added 12 parts of 1-[2,4-dichloro-β-(2,4-dichlorobenzyloxy)phenethyl]-3-phenethylimidazolium bromide. The resulting mixture is heated slowly to reflux temperature and stirred at reflux for 1.25 hours. The mixture is then cooled and evaporated, and the residue is triturated in n-hexane. The latter is decanted and the residual oil is boiled in methyl ethyl ketone, whereupon the desired product is precipitated as a solid. The latter is filtered off and crystallized from dioxane to obtain a purified 1-[2,4-dichloro-β-(2,4-dichlorobenzyloxy)phenethyl]-3-phenethylimidazolium chloride product, m.p. 159.5° C.

後処理

  1. temperatureThe resulting mixture is heated slowly
  2. temperatureto reflux temperature
  3. temperatureat reflux for 1.25 hours
  4. temperatureThe mixture is then cooled
  5. customevaporated
  6. customthe residue is triturated in n-hexane
  7. customThe latter is decanted
  8. customis precipitated as a solid
  9. filtrationThe latter is filtered off
  10. customcrystallized from dioxane

出典と根拠

ORDレコード
ord-9648fd48b6034aa4a838f8a9b8221a2d
出典データセット
uspto-grants-1976_11
特許番号
US03991202

反応ノート

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