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HRID 234130생성일: 2026년 10월 25일

Hydrochloric Acid → 2-Benzothiazolinone, 6-fluoro-

https://huagongshe.com/reaction/234130

반응식

참여 물질

역할이름HCID투입량
반응물Hydrochloric AcidHCID 313—
반응물2-Amino-6-fluorobenzothiazoleHCID 319954—
반응물Sodium NitriteHCID 23668193—
생성물2-Benzothiazolinone, 6-fluoro-HCID 4466785%

반응 조건

온도50 °C

반응 단계

22.4 g of 2-amino-6-fluorobenzothiazole (pure substance content: 97%) and 191.1 g of 30% hydrochloric acid are introduced into a 750 ml pressure vessel at room temperature. The mixture is subsequently heated for 30 minutes at 50° C. and then cooled to 10° C. Then, 46.7 g of aqueous, 40% sodium nitrite solution are metered in at a uniform rate in the course of 1 hour at 10° C., with vigorous stirring. After metering in has ended, stirring of the reaction mixture is continued for 12 hours at 20° C. Excess nitrite is then removed by adding approximately 12.5 g of 18% aqueous urea solution. The reaction vessel is subsequently sealed, and the reaction mixture is heated for 5 hours at 140°-150° C. (pressure approximately 4-5 bar). After the mixture has cooled to 20° C., the gray, crystalline product is filtered off with suction, washed with a small amount of water and dried at 60° C. to constant weight. 18.9 g of 6-fluorobenzothiazol-2-one with a pure substance content of 97.7% are obtained (corresponding to 85% yield). The product which is redissolved under alkaline conditions has a melting point of 188.4° C.

출처 및 근거

DOI10.6084/m9.figshare.5104873.v1
특허 번호US05594145
출처 데이터셋uspto-grants-1997_01
ORD IDord-bdc8c9d26b944fa8a12b80ac476d4bdf
출처 메모uspto-grants-1997_01