반응 #70189

ord-feaa4774383b457f974f91b5b3af3c4a

용매

반응 조건

온도
80°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    농축The reaction mixture was concentrated until methanol
  2. 2
    기타was evaporated
  3. 3
    기타A white solid was obtained
  4. 4
    온도under heating
  5. 5
    온도then cooled with an ice bath
  6. 6
    기타A white precipitate was formed
  7. 7
    여과filtered
  8. 8
    세척washed with water
  9. 9
    기타dried under high vacuum over night

실험 절차

2-Methyl-4-(1-methyl-cyclopropyl)-benzoic acid methyl ester (2.75 g, 13.46 mmol) was treated with methanol and 5 M aqueous sodium hydroxide solution (20.46 ml, 102.32 mmol). This solution was heated to 80° C. for 4 hours. The reaction mixture was concentrated until methanol was evaporated. A white solid was obtained. The solid was dissolved in 50 ml water under heating then cooled with an ice bath; acidified with 10 ml conc. hydrochloric acid. A white precipitate was formed; filtered; washed with water; dried under high vacuum over night to yield 2-Methyl-4-(1-methyl-cyclopropyl)-benzoic acid (2.18 g, 11.46 mmol) MS (ESI) 189.1 (M−H)−

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08536166B2uspto-grants-2013_09