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61350-60-5 → HCID 68961477, 화합물

HRID 1431940
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HRID 1431940 반응식
[Si]([C:5]1[N:6]=NN[CH:9]=1)(C)(C)C.[N:10]1([C:18]([O:20][CH2:21][C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)=[O:19])[CH2:17][CH2:16][CH2:15][C@H:11]1[C:12](Cl)=[O:13]>S1(CCCC1)(=O)=O.[Cl-].[Na+].O>[CH2:21]([O:20][C:18]([N:10]1[CH2:17][CH2:16][CH2:15][CH:11]1[C:12]1[O:13][CH:9]=[CH:5][N:6]=1)=[O:19])[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 1103285461350-60-5HCID 178504166HCID 178504166, 화합물

생성물 1

HCID 68961477HCID 68961477, 화합물

시약·촉매·용매 2

HCID 31347Sulfolane용매2회HCID 57417360Sodium chloride; water용매

실험 절차

To a solution of TMS-triazole (14.17 g, 100.3 mmol, 1 equiv.) in sulfolane (290 mL) at rt under nitrogen, is added dropwise Z-L-Pro-Cl (26.85 g, 100.3 mmol, 1 equiv.) in sulfolane (70 mL). The resulting mixture is stirred at rt for 30 minutes, then the temperature is elevated to 140° C. for 3 hours. After the reaction mixture is cooled to rt, poured into excess brine and extracted with diethyl ether. The diethyl ether extracts are washed with brine, dried over anhydrous Na2SO4, filtered and evaporated. The residue is purified by flash chromatography (DCM:acetone=9:1) to give the title compound as a light yellow oil.

후처리

  1. waitthe temperature is elevated to 140° C. for 3 hours
  2. temperatureAfter the reaction mixture is cooled to rt
  3. extractionextracted with diethyl ether
  4. washThe diethyl ether extracts are washed with brine
  5. dry with materialdried over anhydrous Na2SO4
  6. filtrationfiltered
  7. customevaporated
  8. customThe residue is purified by flash chromatography (DCM:acetone=9:1)

출처 및 근거

ORD 기록
ord-17fe2430fca64e4ab50084c8d37b167a
출처 데이터셋
uspto-grants-2009_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07612059B2

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