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

HRID 1887029노트

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HRID 1887029 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
170 °C

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-df0240a9746e48d5869552fa4a61adf4
출처 데이터셋
uspto-grants-2013_08
특허 번호
US08501738B2

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