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

HRID 548819노트

반응식

HRID 548819 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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]+.

후처리

  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

출처 및 근거

ORD 기록
ord-ddc07c11c9ec4d7ca8a115781183c991
출처 데이터셋
uspto-grants-2011_05
특허 번호
US07943619B2

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