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Trityl chloride → HCID 13471706、化合物

HRID 746320
ノート
印刷プレビュー

反応式

HRID 746320 の反応式
[NH:1]1[CH:5]=[C:4]([C:6]([O:8][CH2:9][CH3:10])=[O:7])[N:3]=[N:2]1.[C:11](Cl)([C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1)([C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1.C(N(CC)CC)C>C(Cl)(Cl)Cl>[C:11]([N:1]1[CH:5]=[C:4]([C:6]([O:8][CH2:9][CH3:10])=[O:7])[N:3]=[N:2]1)([C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)([C:24]1[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=1)[C:18]1[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6456Trityl chlorideHCID 8471TriethylamineHCID 178469944HCID 178469944、化合物

生成物 1

HCID 13471706HCID 13471706、化合物収率 88.8%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

3.47 g of ethyl 1,2,3-triazole-4-carboxylate and 7.55 g of trityl chloride were dissolved in 100 ml of chloroform and 3.77 ml of triethylamine was added dropwise thereto under stirring and cooling in an ice-bath. The resulting mixture was stirred for 30 minutes at room temperature. Chloroform was distilled off and the residue was dissolved in ethyl acetate and the mixture was washed with an aqueous solution of sodium chloride and then dried with sodium sulfate. Ethyl acetate was distilled off and the residue was purified by silica gel column chromatography with benzene and chloroform eluent to give 8.37 g of ethyl N-trityl-1,2,3-triazole-4-carboxylate with mp 201°-203° C.

後処理

  1. temperaturecooling in an ice-bath
  2. stirringThe resulting mixture was stirred for 30 minutes at room temperature
  3. distillationChloroform was distilled off
  4. dissolutionthe residue was dissolved in ethyl acetate
  5. washthe mixture was washed with an aqueous solution of sodium chloride
  6. dry with materialdried with sodium sulfate
  7. distillationEthyl acetate was distilled off
  8. customthe residue was purified by silica gel column chromatography with benzene and chloroform eluent

出典と根拠

ORDレコード
ord-456bae0a376f4d71879ee8edffd5eedb
出典データセット
uspto-grants-1986_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04603198

反応ノート

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