4,6-Dichloro-5-nitropyrimidine → 4-chloro-6-methoxy-5-nitropyrimidine

HRID 1388892ノート

反応式

HRID 1388892 の反応式
[N+:1]([C:4]1[C:5]([Cl:11])=[N:6][CH:7]=[N:8][C:9]=1Cl)([O-:3])=[O:2].C[CH2:13][O-:14].[Na+]>>[Cl:11][C:5]1[C:4]([N+:1]([O-:3])=[O:2])=[C:9]([O:14][CH3:13])[N:8]=[CH:7][N:6]=1

参加物

3

反応物 2

HCID 203124,6-Dichloro-5-nitropyrimidineHCID 2723922Sodium ethoxide

生成物 1

HCID 2522044-chloro-6-methoxy-5-nitropyrimidine収率 98.3%

実験手順

100 g 5-nitro 4,6-dichloropyrimidine are heated in 1000 ml sodium ethylate solution (16.8 g sodium) for 10 hours to 50° C. Then the reaction mixture is evaporated under vacuum and the residue is stirred with water and vacuum treated. Subsequently, it is extracted several times with hot petroleum ether (boiling range 40° to 60° C.). After cooling, the crystals are vacuum treated and dried. 46 g 4-chloro-6-methoxy-5-nitropyrimidine are obtained having a melting point of 65° C.

後処理

  1. customThen the reaction mixture is evaporated under vacuum
  2. additiontreated
  3. extractionSubsequently, it is extracted several times with hot petroleum ether (boiling range 40° to 60° C.)
  4. temperatureAfter cooling
  5. additiontreated
  6. customdried

出典と根拠

ORDレコード
ord-a50f6e391acb4900bcd05d226c670c22
出典データセット
uspto-grants-1984_02
特許番号
US04434167

反応ノート

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