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

HRID 14234ノート

反応式

HRID 14234 の反応式
[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]

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-cdc79e5202b84351980304bc5cd7a27a
出典データセット
uspto-grants-2010_06
特許番号
US07727997B2

反応ノート

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