多聚甲醛 → [3-(trifluoromethyl)-1H-pyrazol-1-yl]methanol

HRID 1982999笔记

反应方程式

HRID 1982999 反应方程式
[F:1][C:2]([F:9])([F:8])[C:3]1[CH:7]=[CH:6][NH:5][N:4]=1.[CH2:10]=[O:11].C(N(CC)CC)C>CC(C)=O>[F:1][C:2]([F:9])([F:8])[C:3]1[CH:7]=[CH:6][N:5]([CH2:10][OH:11])[N:4]=1

参与物

5

反应物 3

HCID 712多聚甲醛HCID 8471三乙胺HCID 18070343-(三氟甲基)吡唑

产物 1

HCID 23149202[3-(trifluoromethyl)-1H-pyrazol-1-yl]methanol收率 86.5%

试剂、催化剂与溶剂 1

HCID 180丙酮溶剂

反应条件

温度
80 °C

实验过程

The mixture of 4.08 g of 3-(trifluoromethyl)-1H-pyrazole, 2.00 g of paraformaldehyde and 1 ml of triethylamine was stirred at 80° C. for 5 hours. After the reaction mixture was cooled to room temperature, acetone was added to the reaction mixture. The mixture was filtered. The filterate was concentrated under reduced pressure. Hexane was added to the residue, and then crystalline was formed. The crystalline was collected to obtain 4.31 g of 3-(trifluoromethyl)-1H-pyrazole-1-ylmethanol.

后处理

  1. temperatureAfter the reaction mixture was cooled to room temperature
  2. filtrationThe mixture was filtered
  3. concentrationThe filterate was concentrated under reduced pressure
  4. additionHexane was added to the residue
  5. customcrystalline was formed
  6. customThe crystalline was collected

来源与证据

ORD记录
ord-1dc556a7a7964805b58ede2195bf92a1
来源数据集
uspto-grants-2009_06
专利号
US07541374B2

反应笔记

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