Dimethyl Sulfoxide → HCID 20194680、化合物

HRID 653410

反応式

HRID 653410 の反応式
Cl[C:2]1[N:7]=[CH:6][C:5]([Cl:8])=[CH:4][N:3]=1.CS(C)=O.[NH2:13][C:14]1[CH:19]=[CH:18][C:17](O)=[C:16]([N+:21]([O-:23])=[O:22])[CH:15]=1.C(=O)([O-])[O-].[K+].[K+]>O>[Cl:8][C:5]1[CH:4]=[N:3][C:2]([C:17]2[CH:18]=[CH:19][C:14]([NH2:13])=[CH:15][C:16]=2[N+:21]([O-:23])=[O:22])=[N:7][CH:6]=1

参加物

6

反応物 4

HCID 679Dimethyl SulfoxideHCID 11430Potassium CarbonateHCID 5906412,5-DichloropyrimidineHCID 34174194-Amino-2-Nitrophenol

生成物 1

HCID 20194680HCID 20194680、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

1.43 g of 2,5-dichloropyrimidine was dissolved in 20 mol of dimethyl sulfoxide. To this solution, a mixture of 1.50 g of 4-amino-2-nitrophenol and 5 ml of water, and 2.69 g of potassium carbonate were added, and the mixture was reacted in the atmosphere of nitrogen gas at a temperature of from 100° to 110° C. for 2 hours. After the completion of the reaction, the reaction product was poured into water, and extracted with methylene chloride. The extract layer was washed with brine and dried over anhydrous sodium sulfate, and purified by silica gel column chromatography, whereby 0.74 g of 4-(5-chloro-2-pyrimidinyl)-3-nitroaniline having a melting point of from 151° to 152° C., was obtained.

後処理

  1. additionwere added
  2. customthe mixture was reacted in the atmosphere of nitrogen gas at a temperature of from 100° to 110° C. for 2 hours
  3. customAfter the completion of the reaction
  4. extractionextracted with methylene chloride
  5. washThe extract layer was washed with brine
  6. dry with materialdried over anhydrous sodium sulfate
  7. custompurified by silica gel column chromatography, whereby 0.74 g of 4-(5-chloro-2-pyrimidinyl)-3-nitroaniline having a melting point of from 151° to 152° C.
  8. customwas obtained

出典と根拠

ORDレコード
ord-d7d16c1e695c4613b2736ebd0cc7678f
出典データセット
uspto-grants-1987_06
特許番号
US04677111

関連ノート

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