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Trityl chloride → HCID 13471706, 화합물

HRID 746320
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HRID 746320 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6456Trityl chlorideHCID 8471TriethylamineHCID 178469944HCID 178469944, 화합물

생성물 1

HCID 13471706HCID 13471706, 화합물수율 88.8%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-456bae0a376f4d71879ee8edffd5eedb
출처 데이터셋
uspto-grants-1986_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04603198

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