تفاعل #167400

معادلة التفاعل

methanol

2-Methyl-acrylic acid

Benzene-1,4-diol

Benzothiazol-6-ylamine

→

product

المردود 27.4%

3-(Benzothiazol-6-ylamino)-2-methyl-propionic Acid

المردود 27.4%

المذيبات

chloroform

toluene

ظروف التفاعل

المعالجة

1. 1
   أخرىThe resulting reaction mass
2. 2
   درجة الحرارةThe reaction mixture was cooled to room temperature
3. 3
   أخرىpartitioned between water and ethyl acetate
4. 4
   غسيلThe organic layer was washed with brine solution
5. 5
   تجفيفdried over Na2SO4
6. 6
   تركيزconcentrated
7. 7
   أخرىto afford the crude product
8. 8
   أخرىPurification by column chromatography on silica gel (0.75% methanol in chloroform)

الإجراء التجريبي

2-Methyl-acrylic acid (0.63 g, 0.00732 mol) and Benzene-1,4-diol (0.029 g, 0.000266 mol) were added to a stirred solution of Benzothiazol-6-ylamine (1 g, 0.00665 mol) in toluene (6 mL) under nitrogen atmosphere. The resulting reaction mass was heated at 70° C. for 72 hours and further at 100° C. for 48 hours. The reaction was monitored by TLC (5% methanol in chloroform). The reaction mixture was cooled to room temperature and partitioned between water and ethyl acetate. The organic layer was washed with brine solution, dried over Na2SO4 and concentrated to afford the crude product. Purification by column chromatography on silica gel (0.75% methanol in chloroform) afforded 0.43 g of the product (26.87% yield).

المصدر