6-Nitroindazole → HCID 178526457, 화합물

반응식

[N+:1]([C:4]1[CH:12]=[C:11]2[C:7]([CH:8]=[N:9][NH:10]2)=[CH:6][CH:5]=1)([O-:3])=[O:2].S(Cl)([Cl:16])(=O)=O>ClCCCl>[Cl:16][C:8]1[C:7]2[C:11](=[CH:12][C:4]([N+:1]([O-:3])=[O:2])=[CH:5][CH:6]=2)[NH:10][N:9]=1

참가 물질

반응 조건

온도: 80 °C

실험 절차

To a solution of 6-nitroindazole (2 mmol) in DCE (5 mL), sulfuryl chloride (10 mmol) was added and the resulting mixture was heated 80° C. for 3-5 h. The reaction mixture was concentrated, added with 5% aqueous Na2CO3 solution (20 mL) and extracted with EtOAc (2×15 mL). The combined organics were then washed with water (20 mL) and brine (20 mL) and dried over anhydrous Na2SO4. Removal of volatiles afforded 3-chloro-6-nitro-1H-indazole as a yellow solid.

후처리

concentrationThe reaction mixture was concentrated
additionadded with 5% aqueous Na2CO3 solution (20 mL)
extractionextracted with EtOAc (2×15 mL)
washThe combined organics were then washed with water (20 mL) and brine (20 mL)
dry with materialdried over anhydrous Na2SO4
customRemoval of volatiles

출처 및 근거

ORD 기록: ord-62054ca5d7a94f238984c26777a25bb4
출처 데이터셋: uspto-grants-2013_02
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US08377983B2

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참가 물질

반응물 2

HCID 242396-Nitroindazole

HCID 24648Sulfuryl chloride

생성물 1

HCID 178526457HCID 178526457, 화합물

시약·촉매·용매 1

HCID 111,2-Dichloroethane용매

반응 조건

온도: 80 °C

실험 절차

후처리

concentrationThe reaction mixture was concentrated
additionadded with 5% aqueous Na2CO3 solution (20 mL)
extractionextracted with EtOAc (2×15 mL)
washThe combined organics were then washed with water (20 mL) and brine (20 mL)
dry with materialdried over anhydrous Na2SO4
customRemoval of volatiles

출처 및 근거

ORD 기록: ord-62054ca5d7a94f238984c26777a25bb4
출처 데이터셋: uspto-grants-2013_02
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US08377983B2

반응 노트

불러오는 중…