تفاعل #710499
ord-1031ba65d9544db5a39cfaecf3b4391c
معادلة التفاعل
[2-chloro-6-(trifluoromethyl)pyridin-3-yl]methanol
pyridinium chlorochromate
→
2-chloro-6-(trifluoromethyl)nicotinaldehyde
المردود 88.3%
المتفاعلات
الكواشف
لا شيء
المذيبات
ظروف التفاعل
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1أخرىAfter completion of reaction, reaction mixture
- 2ترشيحwas filtered through silica gel bed
- 3غسيلwashed the bed with excess 90% ethyl acetate in pet ether and filtrate
- 4تركيزwas concentrated under reduced pressure
الإجراء التجريبي
To a stirred solution of [2-chloro-6-(trifluoromethyl)pyridin-3-yl]methanol (Int-16) (80.0 g, 1.0 eq.) in dichloromethane (700 ml) was added pyridinium chlorochromate (160.0 g, 2.0 eq), silicium dioxide (240 g) at room temperature and stirred for 4 h. The progress of the reaction was monitored by TLC. After completion of reaction, reaction mixture was filtered through silica gel bed and washed the bed with excess 90% ethyl acetate in pet ether and filtrate was concentrated under reduced pressure to get crude 2-chloro-6-(trifluoromethyl)nicotinaldehyde (Int-17) as yellow liquid (70.0 g, 88.3%). GC-MS: m/z 209 ([M]).