Hydrochloric Acid → HCID 316821、化合物

HRID 887600

反応式

HRID 887600 の反応式
[CH3:1][C:2]1[CH:7]=[CH:6][N:5]=[CH:4][N:3]=1.Cl.[N:9](OCC)=[O:10]>CCO>[N:5]1[CH:6]=[CH:7][C:2]([CH:1]=[N:9][OH:10])=[N:3][CH:4]=1

参加物

5

反応条件

温度
0 °C

実験手順

9.14 g (97.11 mmol) of 4-methylpyrimidine was slowly added to a 0° C. solution of 8.75 g HCl in 40 ml EtOH. To this white suspension was added, over 5 min, 61 ml of a 10-20% by weight solution of ethyl nitrite in EtOH. The reaction was stirred at 0° C. for 10 min and then at RT for 2.5 h. The white salt was filtered and dried under vacuum. The salt was dissolved into 20 ml H2O and very slowly treated with about 200 ml saturated aqueous KHCO3. A white solid precipitated out of the purple solution. The solid was filtered and dried under vacuum to yield the titled compound.

後処理

  1. additionTo this white suspension was added, over 5 min
  2. waitat RT for 2.5 h
  3. filtrationThe white salt was filtered
  4. customdried under vacuum
  5. dissolutionThe salt was dissolved into 20 ml H2O
  6. additionvery slowly treated with about 200 ml saturated aqueous KHCO3
  7. customA white solid precipitated out of the purple solution
  8. filtrationThe solid was filtered
  9. customdried under vacuum

出典と根拠

ORDレコード
ord-a7e9d0c8acb0496eaffb383fe0370721
出典データセット
uspto-grants-2012_08
特許番号
US08247430B2

関連ノート

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