تفاعل #725904
ord-e5d59bf5aed247e1bcdef7f0987fedee
معادلة التفاعل
2-(4-Aminophenoxy)propionic acid methyl ester
2-(4-Amino-phenoxy)-propionic acid methyl ester
triethylamine
triphosgene
→
32
المردود 143.8%
2-(4-Isocyanato-phenoxy)-propionic acid methyl ester
المردود 143.8%
المتفاعلات
الكواشف
لا شيء
المذيبات
ظروف التفاعل
درجة الحرارة
75°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1درجة الحرارةmaintained at this temp
- 2درجة الحرارةThe reaction mixture was cooled to room temperature
- 3ترشيحthe solids were filtered off
- 4workup.DISTILLATIONthe toluene was distilled off under vacuum
- 5أخرىto get crude 32, which
- 6workup.DISTILLATIONdistilled
الإجراء التجريبي
To a mixture of 2-(4-Aminophenoxy)propionic acid methyl ester 18 (15 grams, 76.9 mmol) and triethylamine (15.6 g, 154.16 mmol) in toluene (210 ml) under nitrogen atm. was added triphosgene (8.4 g, 28.3 mmol) in one lot. Later the reaction mixture was heated to 75° C. over a period of one hour and maintained at this temp. for 26 hours. The reaction mixture was cooled to room temperature, the solids were filtered off, and the toluene was distilled off under vacuum to get crude 32, which was vacuum distilled to get pure 32 (9 g, 52.9%) as a light yellow syrup.