Potassium Carbonate → 4-(6-Chloro-pyrimidin-4-yloxy)-2-methyl-6-nitro-phenylamine

HRID 1846452노트

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HRID 1846452 반응식
C(=O)([O-])[O-].[K+].[K+].Cl[C:8]1[CH:13]=[C:12]([Cl:14])[N:11]=[CH:10][N:9]=1.[NH2:15][C:16]1[C:21]([N+:22]([O-:24])=[O:23])=[CH:20][C:19]([OH:25])=[CH:18][C:17]=1[CH3:26]>CN(C=O)C>[Cl:14][C:12]1[N:11]=[CH:10][N:9]=[C:8]([O:25][C:19]2[CH:20]=[C:21]([N+:22]([O-:24])=[O:23])[C:16]([NH2:15])=[C:17]([CH3:26])[CH:18]=2)[CH:13]=1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 709434,6-DichloropyrimidineHCID 669782964-Amino-3-methyl-5-nitrophenol

생성물 1

HCID 866639074-(6-Chloro-pyrimidin-4-yloxy)-2-methyl-6-nitro-phenylamine

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
50 °C

실험 절차

1.66 g (12.0 mmol) potassium carbonate were added to 0.922 g (6.00 mmol) 4,6-dichloropyrimidine and 1.11 g (6.60 mmol) 4-amino-3-methyl-5-nitro-phenol in 1.5 mL DMF and the mixture was stirred for 6 h at 50° C. Then the mixture was added to ice water and extracted several times with EtOAc. The combined organic phases were dried on sodium sulphate, evaporated down and purified by flash chromatography. The product-containing fractions were combined and evaporated down. The residue was triturated with EtOAc, suction filtered and dried under HV.

후처리

  1. extractionextracted several times with EtOAc
  2. customThe combined organic phases were dried on sodium sulphate
  3. customevaporated down
  4. custompurified by flash chromatography
  5. customevaporated down
  6. customThe residue was triturated with EtOAc, suction
  7. filtrationfiltered
  8. customdried under HV

출처 및 근거

ORD 기록
ord-1242765a086742be884edd4f3b8e7ebb
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08952014B2

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