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Methanol → 5-bromo-3-methyl-1-(toluene-4-sulfonyl)-1H-indazol-6-ylamine

HRID 1691806
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HRID 1691806 반응식
[CH3:1][C:2]1[C:10]2[C:5](=[CH:6][C:7]([NH2:11])=[CH:8][CH:9]=2)[N:4]([S:12]([C:15]2[CH:20]=[CH:19][C:18]([CH3:21])=[CH:17][CH:16]=2)(=[O:14])=[O:13])[N:3]=1.CO.[Br-:24].[Br-].[Br-].C([N+](CCCC)(CCCC)CCCC)CCC.C([N+](CCCC)(CCCC)CCCC)CCC.C([N+](CCCC)(CCCC)CCCC)CCC>ClCCCl>[Br:24][C:8]1[CH:9]=[C:10]2[C:5](=[CH:6][C:7]=1[NH2:11])[N:4]([S:12]([C:15]1[CH:20]=[CH:19][C:18]([CH3:21])=[CH:17][CH:16]=1)(=[O:14])=[O:13])[N:3]=[C:2]2[CH3:1]
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참가 물질

5

반응물 3

HCID 887MethanolHCID 23500184Tetra-n-butylammonium tribromideHCID 593777823-methyl-1-(toluene-4-sulfonyl)-1H-indazol-6-ylamine

생성물 1

HCID 593778015-bromo-3-methyl-1-(toluene-4-sulfonyl)-1H-indazol-6-ylamine수율 147.7%

시약·촉매·용매 1

HCID 111,2-Dichloroethane용매

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온도
80 °C

실험 절차

3-Methyl-1-(toluene-4-sulfonyl)-1H-indazol-6-ylamine (301 mg, 1.0 mmol) was dissolved in 1,2-dichloroethane (80 ml) and methanol (40 ml) at room temperature. The mixture was heated to 80° C. and then the tetrabutylammonium tribromide (1.0 eq, 482 mg) was added. Stirring was continued for 10 minutes, and then the mixture was partitioned between diethyl ether and saturated aqueous sodium sulfite solution. The organic layer was separated, washed with water, dried over anhydrous sodium sulfate, filtered and concentrated in vacuo. The residue was purified by flash chromatography (gradient 9:1 to 4:1 hexanes/ethyl acetate) to give 5-bromo-3-methyl-1-(toluene-4-sulfonyl)-1H-indazol-6-ylamine (280 mg, 73.7%) as a white powder.

후처리

  1. customat room temperature
  2. customthe mixture was partitioned between diethyl ether and saturated aqueous sodium sulfite solution
  3. customThe organic layer was separated
  4. washwashed with water
  5. dry with materialdried over anhydrous sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo
  8. customThe residue was purified by flash chromatography (gradient 9:1 to 4:1 hexanes/ethyl acetate)

출처 및 근거

ORD 기록
ord-913038bc785744b7840714c7b888a72d
출처 데이터셋
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08153809B2

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