반응 #495809
ord-6d18a7e0852447e48ad0e4650ed05b99
반응 방정식
oxalyl chloride
benzothiophene carboxylic acid
DMF
→
benzo[b]thiophene-3-carbonyl chloride
반응 조건
온도
20°CELSIUS
상세 조건
See reaction.notes.procedure_details.
후처리
- 1농축the reaction mixture is concentrated to 5 volumes
- 2기타to remove the excess of oxalyl chloride
실험 절차
To benzothiophene carboxylic acid (7 g) in MeTHF (6.5 Vols, 45.5 mL) is added a catalytic amount of DMF (0.01 eq.). Then, oxalyl chloride (1.1 eq.) is charged slowly to control the gaz release. After 16 h of stirring at 20° C., the end of the reaction is controlled by HPLC. MeTHF (6.5 Vols) is next added and the reaction mixture is concentrated to 5 volumes to remove the excess of oxalyl chloride. The resulting benzo[b]thiophene-3-carbonyl chloride is stored in a MeTHF solution.