تفاعل #76323

ord-7cc77ebebe164d0780842c4363c5a42a

الكواشف

لا شيء

ظروف التفاعل

درجة الحرارة
100°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىwas placed in a sealed tube
  2. 2
    أخرىgiving a dark solution
  3. 3
    درجة الحرارةThe stirred solution was heated 18 h
  4. 4
    درجة الحرارةcooled
  5. 5
    أخرىto give a dark oil
  6. 6
    أخرىPurification by flash chromatography on silica gel eluting with dichloromethane

الإجراء التجريبي

Ex-588B) A mixture of solid 3-phenoxyaniline (2.96 g, 16 mmol) and 1,1,1-trifluoro-2,3-epoxypropane (1.30 mL, 15.0 mmol) was placed in a sealed tube and heated to 100° C. giving a dark solution. The stirred solution was heated 18 h and cooled to give a dark oil. Purification by flash chromatography on silica gel eluting with dichloromethane gave 3.15 g (71%) of the desired 3-[(N-3-phenoxy-phenyl)amino]-1,1,1-trifluoro-2-propanol product as a colorless oil. Anal. calcd. for C15H14NO2F3.0.05 CH2Cl2: C, 59.92; H, 4.71; N, 4.64. Found: C, 59.92; H, 4.53; N, 4.73. HRMS calcd. 298.1055 [M+H]+, found: 298.1056.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06699898B2uspto-grants-2004_03