تفاعل #51667
ord-ffe6f370f9a649a1b163cc5fc18bcff1
معادلة التفاعل
المتفاعلات
الكواشف
لا شيء
ظروف التفاعل
درجة الحرارة
120°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1درجة الحرارةheated in an oil bath
- 2workup.STIRRINGThe homogeneous solution was stirred at this temperature for 90 minutes
- 3درجة الحرارةto cool to room temperature
- 4أخرىThe flask was immersed in an ice bath
- 5workup.ADDITIONthe suspension of the product
- 6workup.STIRRINGwas stirred at this temperature until all was crystalline
- 7ترشيحFiltration
- 8غسيلwashing well with water
- 9أخرىthorough drying
الإجراء التجريبي
The crystalline N-(2-Chloro-6-methanesulfonylmethyl-phenyl)-2,2,2-trifluoro-acetamide of Step 3 was taken up into 200 ml of 2N solution of sodium hydroxide and stirred and heated in an oil bath heated to 120° C. The homogeneous solution was stirred at this temperature for 90 minutes and slowly allowed to cool to room temperature. The flask was immersed in an ice bath and the suspension of the product was stirred at this temperature until all was crystalline. Filtration, washing well with water and thorough drying afforded 13.96 g of pure crystalline 2-chloro-6-methanesulfonylmethyl-phenylamine (90%).