Potassium Carbonate → HCID 67261255, 화합물

HRID 79371

반응식

HRID 79371 반응식
Cl.Cl[CH2:3][C:4]1[CH:8]=[C:7]([CH3:9])[N:6]([CH3:10])[N:5]=1.[I:11][C:12]1[C:20]2[C:15](=[CH:16][CH:17]=[CH:18][C:19]=2[N+:21]([O-:23])=[O:22])[NH:14][N:13]=1.C([O-])([O-])=O.[K+].[K+]>CN(C=O)C>[CH3:10][N:6]1[C:7]([CH3:9])=[CH:8][C:4]([CH2:3][N:14]2[C:15]3[C:20](=[C:19]([N+:21]([O-:23])=[O:22])[CH:18]=[CH:17][CH:16]=3)[C:12]([I:11])=[N:13]2)=[N:5]1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 669375573-(chloromethyl)-1,5-dimethyl-1H-pyrazole hydrochlorideHCID 178526562HCID 178526562, 화합물

생성물 1

HCID 67261255HCID 67261255, 화합물수율 75.9%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To 3-(chloromethyl)-1,5-dimethyl-1H-pyrazole hydrochloride (5.01 g, 27.7 mmol) in DMF (50 mL) was added 3-iodo-4-nitro-1H-indazole (8.00 g, 27.7 mmol) and K2CO3 (15.3 g, 111 mmol). The reaction mixture was stirred for 20 hours. The mixture was concentrated under reduced pressure to remove most of the DMF. The residue was diluted with DCM (100 mL) and washed with H2O. The organic phase was dried (Na2SO4) and concentrated under reduced pressure. The residue was purified by silica gel chromatography (EtOAc/Hexane 1:3) to provide the product (8.35 g).

후처리

  1. concentrationThe mixture was concentrated under reduced pressure
  2. customto remove most of the DMF
  3. additionThe residue was diluted with DCM (100 mL)
  4. washwashed with H2O
  5. dry with materialThe organic phase was dried (Na2SO4)
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was purified by silica gel chromatography (EtOAc/Hexane 1:3)

출처 및 근거

ORD 기록
ord-ba84414bbc5a4f3185805b3965961618
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08841455B2

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