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Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
HRID 44284생성일: 2026년 10월 24일

Hydrochloric Acid → HCID 66636295, 화합물

https://huagongshe.com/ko/reaction/44284

반응식

참여 물질

역할이름HCID투입량
반응물Hydrochloric AcidHCID 313—
반응물TriethylamineHCID 8471—
반응물Sodium HydroxideHCID 14798—
반응물Ethyl (methylthio)acetateHCID 78199—
반응물Tert-Butyl hypochloriteHCID 521297—
반응물3-(4-Amino-benzyl)-5-(4-chloro-phenyl)-3,6-dihydro-[1,3,4]thiadiazin-2-oneHCID 66636570—
용매AcetonitrileHCID 6342—
용매DichloromethaneHCID 6344—
용매TetrahydrofuranHCID 8028—
생성물HCID 66636295HCID 66636295—

반응 조건

온도-60 °C

반응 단계

To a solution of the compound obtained in Step C (38.27 mmoles), in a mixture of CH3CN (115 ml) and THF (115 ml) at −60° C., ethyl(methylsulphanyl)acetate (45.92 mmoles) is added dropwise under a nitrogen atmosphere. tBuOCl (45.92 mmoles) is added dropwise to the reaction mixture over 20 minutes, keeping the temperature between −60° C. and −55° C. After stirring for 1 hour at −60° C., triethylamine (51.66 mmoles) is added dropwise. The reaction mixture is brought to ambient temperature. 240 ml of DCM and then aqueous 3M HCl solution (340 ml) are added. After stirring for 12 hours at ambient temperature, the reaction mixture is made alkaline (pH 10-11) using 20% aqueous sodium hydroxide solution. After extraction with DCM, the organic phase is washed with saturated aqueous NaCl solution. The organic phase is dried over sodium sulphate, filtered and evaporated to dryness. The product obtained is triturated in ethyl ether, filtered and dried in vacuo to yield the title product which is used directly in the next Step.

출처 및 근거

DOI10.6084/m9.figshare.5104873.v1
특허 번호US08541412B2
출처 데이터셋uspto-grants-2013_09
ORD IDord-721b27c7426a4fe0a4a241c1f831b5ac
출처 메모uspto-grants-2013_09