Formaldehyde → (1-ethyl-1H-1,2,4-triazol-5-yl)methanol

HRID 1887029ノート

反応式

HRID 1887029 の反応式
[CH2:1]([N:3]1[CH:7]=[N:6][CH:5]=[N:4]1)[CH3:2].[CH2:8]=[O:9]>ClCCl>[CH2:1]([N:3]1[C:7]([CH2:8][OH:9])=[N:6][CH:5]=[N:4]1)[CH3:2]

参加物

4

反応物 2

HCID 712FormaldehydeHCID 5193051-Ethyl-1,2,4-triazole

生成物 1

HCID 11412385(1-ethyl-1H-1,2,4-triazol-5-yl)methanol収率 63.2%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
170 °C

実験手順

A mixture of 18a (0.5 g, 5.1 mmol) and paraformaldehyde (0.8 g) were heated at 170° C. for 2 hr under microwave irradiation in a 10-mL tube. The mixture was cooled to room temperature and diluted with dichloromethane (10 mL). The solid was removed by filtration and the filtrate was concentrated under reduced pressure. Two runs (total of 10.3 mmol) were combined and the crude product was purified on an Analogix automated column chromatography system (24 g column, 0-4% MeOH/dichloromethane) to give 410 mg of 26a as a white solid.

後処理

  1. temperatureThe mixture was cooled to room temperature
  2. customThe solid was removed by filtration
  3. concentrationthe filtrate was concentrated under reduced pressure
  4. customthe crude product was purified on an Analogix automated column chromatography system (24 g column, 0-4% MeOH/dichloromethane)

出典と根拠

ORDレコード
ord-df0240a9746e48d5869552fa4a61adf4
出典データセット
uspto-grants-2013_08
特許番号
US08501738B2

反応ノート

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