تفاعل #43430

معادلة التفاعل

3,4,6-trichioropyridazine

2-mercaptoethanol

sodium bicarbonate

dichloromethane

→

2-[(3,6-Dichloro-4 pyridazinyl)thio]ethanol

المذيبات

tetrahydrofuran

triethylamine

ظروف التفاعل

المعالجة

1. 1
   workup.ADDITIONAfter the addition
2. 2
   أخرىthe solid was collected
3. 3
   غسيلwashed with water, ether and pentane
4. 4
   أخرىdried in vacuo
5. 5
   أخرىgiving (22.9 g)
6. 6
   أخرىThe combined aqueous and organic fraction was evaporated to half volume
7. 7
   أخرىgiving further solid, which
8. 8
   غسيلwas washed
9. 9
   أخرىdried as above (5.0 g)

الإجراء التجريبي

A solution of 3,4,6-trichioropyridazine (25 g) in tetrahydrofuran (200 ml) and triethylamine (19 ml) was treated at 0° C. (ice bath cooling) with 2-mercaptoethanol (8.33 ml) over 5 minutes. After the addition was complete, the mixture was stirred at room temperature for 72 hours. The mixture was stirred with aqueous sodium bicarbonate solution and dichloromethane and the solid was collected, washed with water, ether and pentane and dried in vacuo, giving (22.9 g). The combined aqueous and organic fraction was evaporated to half volume giving further solid, which was washed and dried as above (5.0 g). The total yield of solid (27.9 g; 91%) contained some bromo-analogue (5-10%) by NMR.

المصدر