Sodium Iodide → N-2-ethyl-cyclohexylamino-3,4,5-trimethoxy-benzoate-hydrochloride

HRID 596235ノート

反応式

HRID 596235 の反応式
[Na].[CH3:2][O:3][C:4]1[CH:5]=[C:6]([CH:10]=[C:11]([O:15][CH3:16])[C:12]=1[O:13][CH3:14])[C:7]([O-:9])=[O:8].Cl.[Cl:18][CH2:19][CH2:20][NH:21][CH:22]1[CH2:27][CH2:26][CH2:25][CH2:24][CH2:23]1.[I-].[Na+]>CN(C)C=O>[ClH:18].[CH3:19][CH2:20][N:21]([C:10]1[C:11]([O:15][CH3:16])=[C:12]([O:13][CH3:14])[C:4]([O:3][CH3:2])=[CH:5][C:6]=1[C:7]([OH:9])=[O:8])[CH:22]1[CH2:27][CH2:26][CH2:25][CH2:24][CH2:23]1

参加物

5

反応物 3

HCID 5238Sodium IodideHCID 13756691N-(2-chloroethyl)cyclohexanamine hydrochlorideHCID 86734526Sodium 3,4,5-trimethoxy-benzoate

生成物 1

HCID 88821243N-2-ethyl-cyclohexylamino-3,4,5-trimethoxy-benzoate-hydrochloride

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To 1.7 g. of sodium-3,4,5-trimethoxy-benzoate 1.45 g. of N-2-chloroethyl-cyclohexylamine hydrochloride and some sodium iodide crystals are added, whereafter 30 ml. of dimethyl formamide are introduced. After cooling toe precipitated crystals are filtered and the filtrate is evaporated. The residue is recrystallized from 96% of ethanol under clarifying with activated charcoal. Thus N-2-ethyl-cyclohexylamino-3,4,5-trimethoxy-benzoate-hydrochloride is obtained. M.p.: 208°-210° C.

後処理

  1. temperatureAfter cooling toe
  2. customprecipitated crystals
  3. filtrationare filtered
  4. customthe filtrate is evaporated
  5. customThe residue is recrystallized from 96% of ethanol

出典と根拠

ORDレコード
ord-eaf5569218344429b65035dc5a7984e5
出典データセット
uspto-grants-1977_03
特許番号
US04010193

反応ノート

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