Triethylamine → HCID 3753008、化合物

A round-bottom flash was charged with 4-iodo-1-methyl-1H-pyrazole-5-carboxylic acid (297 g, 1.18 mol), DCM (2.97 L), and 1,1′-carbonyldiimidazole (CDI) (207 g, 97% by mass, 1.24 mol). The reaction mixture was stirred at room temperature for 45 min. Ammonium chloride (189 g, 3.53 mol) and triethylamine (498 mL, 3.53 mol) were added and the reaction mixture was stirred at room temperature overnight. The reaction mixture was concentrated in vacuo and the residue was suspended in H2O (˜3 L) and granulated at room temperature for 1 h. The solid was collected via filtration, washed with H2O, and dried in a vacuum oven to afford 4-iodo-1-methyl-1H-pyrazole-5-carboxamide as a colorless solid (222 g, 75% yield).

1. stirringthe reaction mixture was stirred at room temperature overnight
2. concentrationThe reaction mixture was concentrated in vacuo
3. waitgranulated at room temperature for 1 h
4. filtrationThe solid was collected via filtration
5. washwashed with H2O
6. customdried in a vacuum oven

ORDレコード

ord-e3bcfb06889648cbaad8ed66c541d6c7

出典データセット

uspto-grants-2016_01

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US09227956B2