반응 #167400

반응 방정식

methanol

2-Methyl-acrylic acid

Benzene-1,4-diol

Benzothiazol-6-ylamine

→

product

수율 27.4%

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

수율 27.4%

용매

chloroform

toluene

반응 조건

후처리

1. 1
   기타The resulting reaction mass
2. 2
   온도The reaction mixture was cooled to room temperature
3. 3
   기타partitioned between water and ethyl acetate
4. 4
   세척The organic layer was washed with brine solution
5. 5
   건조dried over Na2SO4
6. 6
   농축concentrated
7. 7
   기타to afford the crude product
8. 8
   기타Purification by column chromatography on silica gel (0.75% methanol in chloroform)

실험 절차

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).

출처