Potassium Carbonate → HCID 58748359, 화합물

HRID 1040580노트

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HRID 1040580 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[S:8]([NH:11][CH3:12])(=[O:10])=[O:9].[Cl:13][C:14]1[N:19]=[C:18](Cl)[C:17]([Cl:21])=[CH:16][N:15]=1.C([O-])([O-])=O.[K+].[K+]>CN(C=O)C>[Cl:13][C:14]1[N:19]=[C:18]([NH:1][C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=2[S:8]([NH:11][CH3:12])(=[O:10])=[O:9])[C:17]([Cl:21])=[CH:16][N:15]=1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 2372592,4,5-TrichloropyrimidineHCID 11328402-amino-N-methylbenzene-1-sulfonamide

생성물 1

HCID 58748359HCID 58748359, 화합물수율 50%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
45 °C

실험 절차

A mixture of 2-amino-N-methyl-benzenesulfonamide (2.93, 15.75 mmol), 2,4,5 trichloropyrimidine (2.9 g, 15.84 mmol) and K2CO3 (4.5 g, 32.6 mmol) in dry DMF (25 mL) was stirred at 45° C. for 15 h. The solvent was removed and the residue was taken in water and was extracted twice from ethylacetate. Combined organic was washed with water and brine. After drying solvent was removed. Upon triturating with ether and filtration gave the product 2-(2,5-Dichloro-pyrimidin-4-ylamino)-N-methyl-benzenesulfonamide 7 as a white solid (2.6 g, 50%); 1H NMR (400 MHz, CDCl3) δ9.61 (s, 1H), 8.6 (d=12.89 Hz, 1H), 8.53 (s, 1H), 8.27 (s, 1H), 7.68 (m, 1H), 7.27 (m, 1H0, 1.66 (br s, 1H0, 2.66 (s, 3H).

후처리

  1. customThe solvent was removed
  2. extractionwas extracted twice from ethylacetate
  3. washCombined organic was washed with water and brine
  4. customAfter drying solvent
  5. customwas removed
  6. filtrationUpon triturating with ether and filtration

출처 및 근거

ORD 기록
ord-ec1f0aac33c74e64bcaf031dbb08c3f9
출처 데이터셋
uspto-grants-2013_10
특허 번호
US08552186B2

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