Water → HCID 57746172, 화합물

HRID 2365236노트

반응식

HRID 2365236 반응식
C[Si]([CH2:5][N:6]1[CH:10]=[C:9]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][N:12]=2)[N:8]=[N:7]1)(C)C.O.[F-].C([N+](CCCC)(CCCC)CCCC)CCC>C1COCC1>[CH3:5][N:6]1[CH:10]=[C:9]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][N:12]=2)[N:8]=[N:7]1

참가 물질

5

반응물 3

HCID 962Water2회HCID 2724141Tetrabutylammonium FluorideHCID 67495995HCID 67495995, 화합물

생성물 1

HCID 57746172HCID 57746172, 화합물수율 85%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
0 °C

실험 절차

To a solution of 2-(1-trimethylsilanylmethyl-1H-[1,2,3]triazol-4-yl)-pyridine (6.05 g, 26 mmol) in THF (435 mL) was added water (0.94 mL, 52 mmol) and then tetrabutylammonium fluoride (1 M in THF, 31.2 mL, 31 mmol) was added dropwise at 0° C. The reaction mixture was stirred at 0° C. for 1 h. The resulting mixture was poured into water and then the THF was evaporated. The aqueous layer was then extracted with ethyl acetate and the combined organic extracts washed with brine, dried over sodium sulphate, filtered and evaporated. Purification by chromatography (silica, 0 to 100% ethyl acetate in heptane) afforded the title compound (3.53 g, 85%) as a light brown solid. MS: m/e=161.2 [M+H]+.

후처리

  1. customthe THF was evaporated
  2. extractionThe aqueous layer was then extracted with ethyl acetate
  3. washthe combined organic extracts washed with brine
  4. dry with materialdried over sodium sulphate
  5. filtrationfiltered
  6. customevaporated
  7. customPurification by chromatography (silica, 0 to 100% ethyl acetate in heptane)

출처 및 근거

ORD 기록
ord-474370794d3b41b983f9703b0f1bead7
출처 데이터셋
uspto-grants-2014_04
특허 번호
US08697696B2

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