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

HRID 1846452ノート

反応式

HRID 1846452 の反応式
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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
50 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-1242765a086742be884edd4f3b8e7ebb
出典データセット
uspto-grants-2015_02
特許番号
US08952014B2

反応ノート

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