Sodium Hydroxide → HCID 22322113、化合物

HRID 1266319

反応式

HRID 1266319 の反応式
[CH2:1]([N:8]([S:25]([C:28]1[CH:33]=[CH:32][C:31]([O:34][CH3:35])=[CH:30][CH:29]=1)(=[O:27])=[O:26])[C:9]1[C:14]([C:15]([O:17]CC)=[O:16])=[CH:13][N:12]=[C:11]2[N:20]([CH3:24])[N:21]=[C:22]([CH3:23])[C:10]=12)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[OH-].[Na+]>O1CCCC1CO>[CH2:1]([N:8]([S:25]([C:28]1[CH:29]=[CH:30][C:31]([O:34][CH3:35])=[CH:32][CH:33]=1)(=[O:27])=[O:26])[C:9]1[C:14]([C:15]([OH:17])=[O:16])=[CH:13][N:12]=[C:11]2[N:20]([CH3:24])[N:21]=[C:22]([CH3:23])[C:10]=12)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 22322112Ethyl 4-[benzyl-(4-methoxybenzenesulfonyl)amino]-1,3-dimethyl-1H-pyrazolo[3,4-b] pyridine-5-carboxylate

生成物 1

HCID 22322113HCID 22322113、化合物

試薬・触媒・溶媒 1

HCID 7360Tetrahydrofurfuryl alcohol溶媒

反応条件

温度
70 °C

実験手順

A mixture of 0.48 g (0.97 mmol) of ethyl 4-[benzyl-(4-methoxybenzenesulfonyl) amino]-1,3-dimethyl-1H-pyrazolo[3,4-b]pyridine-5-carboxylate and 0.29 ml of ION NaOH in 4 ml of tetrahydrofuran-methanol (1:1) was heated in an oil bath at 70° C. for 2 hours and the solvent removed under vacuum. The residue was dissolved in 20 ml of H2O and the solution extracted with 10 ml of diethyl ether. To the aqucous layer was added 2N citric acid (pH 4-5) and the precipitated solid filtered and washed with H2O to give a white solid which was dried under vacuum overnight to give crystals, mp 165-167° C.

後処理

  1. customthe solvent removed under vacuum
  2. dissolutionThe residue was dissolved in 20 ml of H2O
  3. extractionthe solution extracted with 10 ml of diethyl ether
  4. additionTo the aqucous layer was added 2N citric acid (pH 4-5)
  5. filtrationthe precipitated solid filtered
  6. washwashed with H2O
  7. customto give a white solid which
  8. customwas dried under vacuum overnight
  9. customto give crystals, mp 165-167° C.

出典と根拠

ORDレコード
ord-62b22f4a47c745a4a02c6acdab6c54ac
出典データセット
uspto-grants-2003_04
特許番号
US06548524B2

関連ノート

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