Ammonium fluoride → 5-Methyl-1H-1,2,4-triazole-1-propanol

HRID 454114노트

반응식

HRID 454114 반응식
[F-].[NH4+].C([Si](C)(C)[O:8][CH2:9][CH2:10][CH2:11][N:12]1[C:16]([CH3:17])=[N:15][CH:14]=[N:13]1)(C)(C)C>CO>[CH3:17][C:16]1[N:12]([CH2:11][CH2:10][CH2:9][OH:8])[N:13]=[CH:14][N:15]=1

참가 물질

4

반응물 2

HCID 25516Ammonium fluorideHCID 220308553-(Tertbutyldimethylsilyloxy)-1-(5-methyl-[1,2,4]-triazol-1-yl)propane

생성물 1

HCID 220306985-Methyl-1H-1,2,4-triazole-1-propanol수율 92.3%

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

To a solution of ammonium fluoride (10.4 g, 280 mmol) in methanol (110 ml) was added a solution of 3-(tertbutyldimethylsilyloxy)-1-(5-methyl-[1,2,4]-triazol-1-yl)propane (7.2 g, 28 mmol) in methanol (30 ml). The mixture was refluxed for 4.5 hours. After cooling, silica (100 g) was added and the volatiles were removed under vacuum. The residue was added onto a column of silica and eluted with a mixture of methylene chloride/ethyl acetate (1/1) followed by methylene chloride/methanol (9/1) to give 3-(5-methyl-[1,2,4]-triazol-1-yl)propan-1-ol (3.65 g, 92%).

후처리

  1. temperatureThe mixture was refluxed for 4.5 hours
  2. temperatureAfter cooling
  3. additionsilica (100 g) was added
  4. customthe volatiles were removed under vacuum
  5. additionThe residue was added onto a column of silica
  6. washeluted with a mixture of methylene chloride/ethyl acetate (1/1)

출처 및 근거

ORD 기록
ord-32a6c46cad244fe7be5ad11705e809f1
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08492560B2

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