Sodium Iodide → HCID 178498267、化合物

HRID 726253

反応式

HRID 726253 の反応式
[OH:1][C:2]1[CH:11]=[CH:10][C:5]([C:6]([O:8][CH3:9])=[O:7])=[CH:4][CH:3]=1.Cl.Cl[CH2:14][CH2:15][C:16]1[N:17]=[CH:18][NH:19][CH:20]=1.C(=O)([O-])[O-].[K+].[K+].[I-].[Na+]>CN(C)C=O.C(Cl)(Cl)Cl.CO.C(Cl)(Cl)Cl>[C:6]([C:5]1[CH:4]=[CH:3][C:2]([O:1][CH2:14][CH2:15][C:16]2[N:17]=[CH:18][NH:19][CH:20]=2)=[CH:11][CH:10]=1)([O:8][CH3:9])=[O:7]

参加物

8

反応物 4

HCID 5238Sodium IodideHCID 7456MethylparabenHCID 11430Potassium CarbonateHCID 1784785704-(2-chloroethyl)-1H-imidazole hydrochloride

生成物 1

HCID 178498267HCID 178498267、化合物

試薬・触媒・溶媒 3

HCID 6212Chloroform溶媒HCID 6228Dimethylformamide溶媒HCID 21584188Chloroform methanol溶媒

実験手順

228 mg (1.5 mmol) of methyl 4-hydroxybenzoate, 251 mg (1.5 mmol) of 4-[2-chloroethyl]-1H-imidazole hydrochloride, 500 mg (3.6 mmol) of potassium carbonate and sodium iodide (catalyst) are stirred at 80° C. for 3 days in 5 ml of dimethylformamide. The reaction mixture is cooled and filtered and the filtrate is evaporated under reduced pressure to give an oily residue which is subjected to column chromatography (using, as first eluent, chloroform and, as second eluent, a 95/5 chloroform/methanol mixture). The product is purified by preparative high performance liquid chromatography and crystallized from water; M.p.: 116°-118° C.

後処理

  1. temperatureThe reaction mixture is cooled
  2. filtrationfiltered
  3. customthe filtrate is evaporated under reduced pressure
  4. customto give an oily residue which
  5. customThe product is purified by preparative high performance liquid chromatography
  6. customcrystallized from water

出典と根拠

ORDレコード
ord-de1c05e228e64aefb3975d839f8ae725
出典データセット
uspto-grants-1998_01
特許番号
US05708171

関連ノート

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