Tetrahydrofuran → 2-(Dipropylamino)-6-methylpyrimidine-4-carboxylic acid

HRID 14234

반응식

HRID 14234 반응식
[CH2:1]([N:4]([CH2:16][CH2:17][CH3:18])[C:5]1[N:10]=[C:9]([C:11]([O:13]C)=[O:12])[CH:8]=[C:7]([CH3:15])[N:6]=1)[CH2:2][CH3:3].C1COCC1.O.[OH-].[Li+]>CO.O>[CH2:16]([N:4]([CH2:1][CH2:2][CH3:3])[C:5]1[N:10]=[C:9]([C:11]([OH:13])=[O:12])[CH:8]=[C:7]([CH3:15])[N:6]=1)[CH2:17][CH3:18]

참가 물질

6

반응물 3

HCID 8028TetrahydrofuranHCID 168937Lithium hydroxide, monohydrateHCID 21086142Methyl 2-(dipropylamino)-6-methylpyrimidine-4-carboxylate

생성물 1

HCID 210854602-(Dipropylamino)-6-methylpyrimidine-4-carboxylic acid수율 82.6%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

실험 절차

To methyl 2-(dipropylamino)-6-methylpyrimidine-4-carboxylate (0.450 g, 1.79 mmol) in MeOH (2 mL), water (1 mL), and THF (1 mL) was added lithium hydroxide monohydrate (0.113 g, 2.68 mmol). The mixture was stirred at room temperature for 1 h and then MeOH and THF were removed under reduced pressure. The pH of the residue was adjusted to approximately 5 and the resulting mixture was extracted with dichloromethane, dried over sodium sulfate, and concentrated to give 2-(dipropylamino)-6-methylpyrimidine-4-carboxylic acid (0.351 g) as a yellow solid.

후처리

  1. customMeOH and THF were removed under reduced pressure
  2. extractionthe resulting mixture was extracted with dichloromethane
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated

출처 및 근거

ORD 기록
ord-cdc79e5202b84351980304bc5cd7a27a
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07727997B2

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