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

HRID 454114ノート

反応式

HRID 454114 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

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%).

後処理

  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)

出典と根拠

ORDレコード
ord-32a6c46cad244fe7be5ad11705e809f1
出典データセット
uspto-grants-2013_07
特許番号
US08492560B2

反応ノート

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