Potassium Carbonate → 2-(4-methoxy-7-(3-pivalamido-1H-1,2,4-triazol-1-yl)-1H-pyrrolo[2,3-c]pyridin-3-yl)-2-oxoacetic acid

HRID 1157788ノート

反応式

HRID 1157788 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[N:7][C:6]([N:9]2[CH:13]=[N:12][C:11]([NH:14][C:15](=[O:20])[C:16]([CH3:19])([CH3:18])[CH3:17])=[N:10]2)=[C:5]2[NH:21][CH:22]=[C:23]([C:24](=[O:29])[C:25]([O:27]C)=[O:26])[C:4]=12.C([O-])([O-])=O.[K+].[K+]>O.CO>[CH3:1][O:2][C:3]1[CH:8]=[N:7][C:6]([N:9]2[CH:13]=[N:12][C:11]([NH:14][C:15](=[O:20])[C:16]([CH3:19])([CH3:18])[CH3:17])=[N:10]2)=[C:5]2[NH:21][CH:22]=[C:23]([C:24](=[O:29])[C:25]([OH:27])=[O:26])[C:4]=12

参加物

5

反応物 2

HCID 11430Potassium CarbonateHCID 68694028methyl 2-(4-methoxy-7-(3-pivalamido-1H-1,2,4-triazol-1-yl)-1H-pyrrolo[2,3-c]pyridin-3-yl)-2-oxoacetate

生成物 1

HCID 595114512-(4-methoxy-7-(3-pivalamido-1H-1,2,4-triazol-1-yl)-1H-pyrrolo[2,3-c]pyridin-3-yl)-2-oxoacetic acid収率 78%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

To a mixture of methyl 2-(4-methoxy-7-(3-pivalamido-1H-1,2,4-triazol-1-yl)-1H-pyrrolo[2,3-c]pyridin-3-yl)-2-oxoacetate (40 mg, 0.100 mmol) in water (1 mL) and MeOH (1 mL) was added K2CO3 (83 mg, 0.599 mmol) at room temperature. The reaction mixture was stirred overnight at room temperature. MeOH was removed under reduced pressure. The water layer was acidified to PH=5-6 using 1N HCl and concentrated under reduced pressure. The resulting residue was washed with water, filtered and dried to give 2-(4-methoxy-7-(3-pivalamido-1H-1,2,4-triazol-1-yl)-1H-pyrrolo[2,3-c]pyridin-3-yl)-2-oxoacetic acid (30 mg, 78%) as white solid. LCMS: m/e 387.18 (M+H)+, ret time 2.46 min (method 4).

後処理

  1. customMeOH was removed under reduced pressure
  2. concentrationconcentrated under reduced pressure
  3. washThe resulting residue was washed with water
  4. filtrationfiltered
  5. customdried

出典と根拠

ORDレコード
ord-3f0e307d6fac4b3f9aca4f94dd373572
出典データセット
uspto-grants-2010_10
特許番号
US07807676B2

反応ノート

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