Lawesson's reagent → HCID 86721241, 화합물
반응식
[Br:1][C:2]1[N:6]([C:7]([CH3:10])([CH3:9])[CH3:8])[N:5]=[CH:4][C:3]=1[C:11]([NH2:13])=O.COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:23])=CC=1>C1COCC1>[Br:1][C:2]1[N:6]([C:7]([CH3:10])([CH3:9])[CH3:8])[N:5]=[CH:4][C:3]=1[C:11](=[S:23])[NH2:13]참가 물질
4
실험 절차
A solution of the compound (3.59 g, 14.59 mmol) obtained in step 4 and Lawesson's reagent (5.31 g, 13.13 mmol) in THF (60 mL) was stirred at 60° C. for 2 hr. The reaction mixture was concentrated under reduced pressure, and the residue was purified by NH-silica gel column chromatography (solvent gradient; 2→50% ethyl acetate/hexane) to give 5-bromo-1-tert-butyl-1H-pyrazole-4-carbothioamide (2.8 g, 10.68 mmol, 73%) as a pale-yellow powder.
후처리
- concentrationThe reaction mixture was concentrated under reduced pressure
- customthe residue was purified by NH-silica gel column chromatography (solvent gradient; 2→50% ethyl acetate/hexane)
출처 및 근거
- ORD 기록
- ord-88138da572ba4f06818463283d643776
- 출처 데이터셋
- uspto-grants-2015_10
- 특허 번호
- US09156837B2
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