Iodine → HCID 178506076, 화합물

HRID 1671280노트

반응식

HRID 1671280 반응식
[OH-].[K+].[I:3]I.[F:5][C:6]([F:17])([F:16])[C:7]1[CH:15]=[C:14]2[C:10]([CH:11]=[N:12][NH:13]2)=[CH:9][CH:8]=1.S([O-])([O-])(=O)=S.[Na+].[Na+]>CN(C)C=O>[F:17][C:6]([F:5])([F:16])[C:7]1[CH:15]=[C:14]2[C:10]([C:11]([I:3])=[N:12][NH:13]2)=[CH:9][CH:8]=1

참가 물질

6

반응물 4

HCID 807IodineHCID 14797Potassium HydroxideHCID 24477Sodium ThiosulfateHCID 214555996-(trifluoromethyl)-1H-indazole

생성물 1

HCID 178506076HCID 178506076, 화합물수율 83.3%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

Potassium hydroxide (73 mg, manufactured by Wako Pure Chemical Industries, Ltd.) and iodine (330 mg, manufactured by Kanto Chemical Co., Inc.) were added to a solution of 6-(trifluoromethyl)-1H-indazole (121 mg) synthesized according to the literature (Shoji, et al., Tetrahedron Lett., 2004, 45, 1769-1772) in N,N-dimethylformamide (6.5 mL, manufactured by Kanto Chemical Co., Inc.), and the mixture was stirred for 3 hours at room temperature. An aqueous solution of sodium thiosulfate (20 mL) was added to the reaction solution, and the mixture was extracted with ethyl acetate (3×20 mL), washed with brine (40 mL), and dried (MgSO4). The solvent was then evaporated. The resulting residue was purified by silica gel column chromatography (hexane:ethyl acetate=9:1), to give 169 mg of the title compound. LC-MS: HPLC retention time 4.46 minutes, m/z 313 (M+H), condition B-1.

후처리

  1. customsynthesized
  2. extractionthe mixture was extracted with ethyl acetate (3×20 mL)
  3. washwashed with brine (40 mL)
  4. dry with materialdried (MgSO4)
  5. customThe solvent was then evaporated
  6. customThe resulting residue was purified by silica gel column chromatography (hexane:ethyl acetate=9:1)

출처 및 근거

ORD 기록
ord-003d651ce844454287ad544234d9347d
출처 데이터셋
uspto-grants-2011_08
특허 번호
US07994202B2

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