Sodium Bicarbonate → n-[6-(5-Methyl-3-phenyl-isoxazol-4-ylmethoxy)-pyridazin-3-yl]-acetamide

HRID 548819ノート

反応式

HRID 548819 の反応式
[C:1]([N:4]([C:8]1[N:9]=[N:10][C:11]([O:14][CH2:15][C:16]2[C:17]([C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)=[N:18][O:19][C:20]=2[CH3:21])=[CH:12][CH:13]=1)C(=O)C)(=[O:3])[CH3:2].C(=O)(O)[O-].[Na+]>CO>[CH3:21][C:20]1[O:19][N:18]=[C:17]([C:22]2[CH:23]=[CH:24][CH:25]=[CH:26][CH:27]=2)[C:16]=1[CH2:15][O:14][C:11]1[N:10]=[N:9][C:8]([NH:4][C:1](=[O:3])[CH3:2])=[CH:13][CH:12]=1

参加物

4

反応物 2

HCID 516892Sodium BicarbonateHCID 67157632N-Acetyl-N-[6-(5-methyl-3-phenyl-isoxazol-4-ylmethoxy)-pyridazin-3-yl]-acetamide

生成物 1

HCID 67157871n-[6-(5-Methyl-3-phenyl-isoxazol-4-ylmethoxy)-pyridazin-3-yl]-acetamide収率 65%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A solution of N-acetyl-N-[6-(5-methyl-3-phenyl-isoxazol-4-ylmethoxy)-pyridazin-3-yl]-acetamide (70 mg, 0.19 mmol) in methanol (2 mL) was treated with sodium bicarbonate (1 spatula) and stirred at room temperature for 16 h. The solvent was evaporated and the residue was extracted (dichloromethane/water). The organic phase was dried over sodium sulfate and concentrated. Crystallization of the residue from diisopropylether afforded the title compound as a light brown solid (40 mg, 65%). MS: m/e=325.4 [M+H]+.

後処理

  1. customThe solvent was evaporated
  2. extractionthe residue was extracted (dichloromethane/water)
  3. dry with materialThe organic phase was dried over sodium sulfate
  4. concentrationconcentrated
  5. customCrystallization of the residue from diisopropylether

出典と根拠

ORDレコード
ord-ddc07c11c9ec4d7ca8a115781183c991
出典データセット
uspto-grants-2011_05
特許番号
US07943619B2

反応ノート

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