7-chloro-2,3,4,5-tetrahydro-1-benzothiepin-5-one synthesis
- Product Name:7-chloro-2,3,4,5-tetrahydro-1-benzothiepin-5-one
- CAS Number:30484-10-7
- Molecular formula:C10H9ClOS
- Molecular Weight:212.7
29193-63-3
12 suppliers
inquiry
30484-10-7
4 suppliers
inquiry
Yield:30484-10-7 74.7%
Reaction Conditions:
with polyphosphoric acid for 2 h;
Steps:
5.2 (2) Synthesis of 7-chloro-1-benzothiazepine-one
4-(4-Chlorophenylthio)butyric acid (0.6238 g, 2.70 mmol) and polyphosphoric acid (PPA, 30 g) were weighed into a three-necked flask.After heating at 120 ° C for 2 h with mechanical stirring, the reaction was quenched with ice cubes;The reaction was extracted three times with 25 mL of ethyl acetate.Wash with 5% NaOH and wash with water;The organic layer was taken, dried over anhydrous magnesiumThe T product had a Rf value of 0.658 (TLC, n-hexane-ethyl acetate (95:5)).The crude product is separated by column chromatography and eluted with a developing solvent of n-hexane-ethyl acetate (99:1 to 8:2).The silica gel used had a particle size of 200 to 300 mesh, and the product was obtained in 0.4291 g, and the yield was 74.7%.
References:
CN108640901,2018,A Location in patent:Paragraph 0103; 0109; 0110; 0111
106-54-7
246 suppliers
$10.00/5g
30484-10-7
4 suppliers
inquiry