Sodium Hydroxide → 2-(4-Ethyl-2-(piperidin-1-yl)-6-p-tolylpyrimidin-5-yl)pentanoic acid

HRID 1399740ノート

反応式

HRID 1399740 の反応式
[CH2:1]([C:3]1[C:8]([CH:9]([CH2:14][CH2:15][CH3:16])[C:10]([O:12]C)=[O:11])=[C:7]([C:17]2[CH:22]=[CH:21][C:20]([CH3:23])=[CH:19][CH:18]=2)[N:6]=[C:5]([N:24]2[CH2:29][CH2:28][CH2:27][CH2:26][CH2:25]2)[N:4]=1)[CH3:2].[OH-].[Na+]>CO>[CH2:1]([C:3]1[C:8]([CH:9]([CH2:14][CH2:15][CH3:16])[C:10]([OH:12])=[O:11])=[C:7]([C:17]2[CH:18]=[CH:19][C:20]([CH3:23])=[CH:21][CH:22]=2)[N:6]=[C:5]([N:24]2[CH2:25][CH2:26][CH2:27][CH2:28][CH2:29]2)[N:4]=1)[CH3:2]

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 66955305Methyl 2-(4-ethyl-2-(piperidin-1-yl)-6-p-tolylpyrimidin-5-yl)pentanoate

生成物 1

HCID 669556412-(4-Ethyl-2-(piperidin-1-yl)-6-p-tolylpyrimidin-5-yl)pentanoic acid収率 74.4%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

This compound was prepared according to general method D from methyl 2-(4-ethyl-2-(piperidin-1-yl)-6-p-tolylpyrimidin-5-yl)pentanoate (0.085 g; 0.215 mmol), sodium hydroxide 10N (0.15 mL; 1.50 mmol) in methanol (1.5 mL) at 60° C. for 18 h. The reaction mixture was concentrated under reduced pressure, the residue was dissolved in water and extracted with diethyl ether. The pH of the aqueous layer was adjusted between 2 and 3 by addition of a solution of hydrochloric acid 6N until a precipitate was formed. The suspension was extracted twice with ethyl acetate and the combined organic layers were dried over sodium sulfate and concentrated under reduced pressure to give 0.061 g (74%)of the title compound.

後処理

  1. customThis compound was prepared
  2. concentrationThe reaction mixture was concentrated under reduced pressure
  3. dissolutionthe residue was dissolved in water
  4. extractionextracted with diethyl ether
  5. additionThe pH of the aqueous layer was adjusted between 2 and 3 by addition of a solution of hydrochloric acid 6N until a precipitate
  6. customwas formed
  7. extractionThe suspension was extracted twice with ethyl acetate
  8. dry with materialthe combined organic layers were dried over sodium sulfate
  9. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-a71d7d7132814a2c995e582377b3cb10
出典データセット
uspto-grants-2014_12
特許番号
US08906906B2

反応ノート

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