반응 #1687629

ord-7657e5b7bf7749b5ade477c43dc5633b

반응 방정식

CC(=O)CNC(=O)c1cccnc1
73
CC(=O)CNC(=O)c1cccnc1
N-Acetylmethyl-nicotinamide
N
ammonia
Cc1cnc(-c2cccnc2)o1
74
Cc1cnc(-c2cccnc2)o1
5-Methyl-2-(3-pyridyl)-oxazole

반응 조건

온도
120°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도After cooling the mixture
  2. 2
    workup.ADDITIONwas poured over ice
  3. 3
    추출Extraction with 3×400 ml of dichloromethane
  4. 4
    건조drying of the combined organic phase over magnesium sulphate, and removal of the solvent in vacuo

실험 절차

A mixture of 20 g (0.110 mol) of 73 and 100 ml of conc. sulphuric acid was heated to 120° C. for 4 h. After cooling the mixture was poured over ice followed by basification with ammonia. Extraction with 3×400 ml of dichloromethane, drying of the combined organic phase over magnesium sulphate, and removal of the solvent in vacuo gave crude 74 as a red oil, which was sufficiently pure. Yield: 17 g (0.100 mol, 97%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: USRE036374uspto-grants-1999_11