Potassium Carbonate → HCID 67261255、化合物

HRID 79371

反応式

HRID 79371 の反応式
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

参加物

5

反応物 3

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

生成物 1

HCID 67261255HCID 67261255、化合物収率 75.9%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-ba84414bbc5a4f3185805b3965961618
出典データセット
uspto-grants-2014_09
特許番号
US08841455B2

関連ノート

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