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Sodium Hydroxide → HCID 19018484、化合物

HRID 1109979
ノート
印刷プレビュー

反応式

HRID 1109979 の反応式
[CH3:1][O:2][C:3]1[N:8]=[C:7]([CH3:9])[N:6]=[C:5]([C:10]([O:12]C)=[O:11])[CH:4]=1.[OH-].[Na+]>O.CO>[CH3:1][O:2][C:3]1[N:8]=[C:7]([CH3:9])[N:6]=[C:5]([C:10]([OH:12])=[O:11])[CH:4]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 14798Sodium HydroxideHCID 19018473Methyl 6-methoxy-2-methylpyrimidine-4-carboxylate

生成物 1

HCID 19018484HCID 19018484、化合物収率 43.4%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒2 回HCID 962Water溶媒

実験手順

62.6 g of methyl 6-methoxy-2-methylpyrimidine-4-carboxylate are added to a stirred solution of 14.4 g of sodium hydroxide in 100 ml of water and 350 ml of methanol and stirring is continued until hydrolysis is complete (TLC checking). 200 ml of methanol are added to the reaction mixture, and the sodium salt is filtered off with suction and then washed with methanol/diethyl ether (1:1) on the suction filter. The filter residue (59.3 g; melting point above 265° C.) dried in vacuo at 50° C. is introduced in portions into a solution of 24.5 g of acetyl chloride in 300 ml of methanol. The mixture is then stirred at room temperature for 1/2 h, the solid is filtered off with suction and the filter residue is then washed with abs. methanol. The filtrate is concentrated in vacuo on a rotary evaporator and the residue is dried at high vacuum. 25.1 g of 6-methoxy-2-methylpyrimidine-4-carboxylic acid of melting point 184°-188° C. (dec.) are obtained in this way.

後処理

  1. customis continued until hydrolysis
  2. filtrationthe sodium salt is filtered off with suction
  3. washwashed with methanol/diethyl ether (1:1) on the suction
  4. filtrationfilter
  5. customThe filter residue (59.3 g; melting point above 265° C.) dried in vacuo at 50° C.
  6. additionis introduced in portions into a solution of 24.5 g of acetyl chloride in 300 ml of methanol
  7. stirringThe mixture is then stirred at room temperature for 1/2 h
  8. filtrationthe solid is filtered off with suction
  9. washthe filter residue is then washed with abs
  10. concentrationThe filtrate is concentrated in vacuo on a rotary evaporator
  11. customthe residue is dried at high vacuum

出典と根拠

ORDレコード
ord-5a46970342f343eeb7c119e9e501e0b2
出典データセット
uspto-grants-1994_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05324710

反応ノート

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