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Sodium Hydroxide → HCID 19018484, 화합물

HRID 1109979
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HRID 1109979 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

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

생성물 1

HCID 19018484HCID 19018484, 화합물수율 43.4%

시약·촉매·용매 2

HCID 887Methanol용매2회HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-5a46970342f343eeb7c119e9e501e0b2
출처 데이터셋
uspto-grants-1994_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05324710

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