Nitric Acid → (4-ethyl-4H-1,2,4-triazol-3-yl)methanol

HRID 856643ノート

反応式

HRID 856643 の反応式
[N+]([O-])(O)=O.N([O-])=O.[Na+].[OH:9][CH2:10][C:11]1[N:15]([CH2:16][CH3:17])[C:14](S)=[N:13][N:12]=1.C(=O)([O-])[O-].[Na+].[Na+]>O>[CH2:16]([N:15]1[CH:14]=[N:13][N:12]=[C:11]1[CH2:10][OH:9])[CH3:17]

参加物

6

反応物 4

HCID 944Nitric AcidHCID 10340Sodium CarbonateHCID 23668193Sodium NitriteHCID 178462988HCID 178462988、化合物

生成物 1

HCID 22938611(4-ethyl-4H-1,2,4-triazol-3-yl)methanol収率 76.8%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a mixture of 90% nitric acid (15 ml) and water (22 ml) was added sodium nitrite (0.06 g) and then 3-hydroxymethyl-5-mercapto-4-ethyl-4H-1,2,4-triazole (7.5 g) was slowly added for 0.5 hours at 45° C. After allowing the mixture to be cooled to room temperature, sodium carbonate was slowly added thereto to adjust pH to 7 at 0° C. The reaction mixture was concentrated under reduced pressure, methanol was added to the residue, and the precipitates were removed by filtration. The mixture was concentrated under reduced pressure, and the obtained residue was separated and purified by column chromatography (ethanol:ethyl acetate 2:1), to give 4-ethyl-3-hydroxymethyl-4H-1,2,4-triazole (4.60 g) as brown oil.

後処理

  1. customto adjust pH to 7 at 0° C
  2. concentrationThe reaction mixture was concentrated under reduced pressure, methanol
  3. additionwas added to the residue
  4. customthe precipitates were removed by filtration
  5. concentrationThe mixture was concentrated under reduced pressure
  6. customthe obtained residue was separated
  7. custompurified by column chromatography (ethanol:ethyl acetate 2:1)

出典と根拠

ORDレコード
ord-9bde39f0164e4e79b0adf9981279ccc0
出典データセット
uspto-grants-2007_08
特許番号
US07262185B2

反応ノート

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