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Hydrochloric Acid → HCID 42611021, 화합물

HRID 1517306
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HRID 1517306 반응식
Cl([O-])=O.[Na+].[Cl:5][C:6]1[CH:7]=[C:8]([O:31][CH2:32][CH:33]=[O:34])[CH:9]=[N:10][C:11]=1[O:12][C:13]1[CH:14]=[C:15]2[C:20](=[CH:21][CH:22]=1)[N:19]=[CH:18][N:17]=[C:16]2[NH:23][C:24]1[CH:29]=[N:28][C:27]([CH3:30])=[CH:26][N:25]=1.CC(=CC)C.P([O-])(O)(O)=[O:41].[Na+].Cl>CC(O)(C)C.O>[Cl:5][C:6]1[CH:7]=[C:8]([O:31][CH2:32][C:33]([OH:41])=[O:34])[CH:9]=[N:10][C:11]=1[O:12][C:13]1[CH:14]=[C:15]2[C:20](=[CH:21][CH:22]=1)[N:19]=[CH:18][N:17]=[C:16]2[NH:23][C:24]1[CH:29]=[N:28][C:27]([CH3:30])=[CH:26][N:25]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 5

HCID 313Hydrochloric AcidHCID 105532-Methyl-2-buteneHCID 23668197Sodium ChloriteHCID 23672064Monosodium phosphateHCID 86645904{[5-Chloro-6-({4-[(5-methylpyrazin-2-yl)amino]quinazolin-6-yl}oxy)pyridin-3-yl]oxy}acetaldehyde

생성물 1

HCID 42611021HCID 42611021, 화합물수율 77%

시약·촉매·용매 2

HCID 962Water용매HCID 6386tert-Butanol용매

실험 절차

Sodium chlorite (30 mg, 0.33 mmol) was added to a water (0.3 ml)/2-methyl-2-propanol (1.2 ml) mixed solution of {[5-chloro-6-({4-[(5-methylpyrazin-2-yl)amino]quinazolin-6-yl}oxy)pyridin-3-yl]oxy}acetaldehyde (50 mg, 0.11 mmol) obtained in Example 32, 2-methyl-2-butene (0.051 ml, 0.48 mmol) and sodium dihydrogenphosphate (13 mg, 0.11 mmol), and the reaction solution was stirred at room temperature for 1 hour. Aqueous 1 N hydrochloric acid solution was added to the reaction solution, and extracted with chloroform/methanol (9:1). The organic layer was dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The obtained residue was recrystallized from ethyl acetate to obtain the entitled compound (37 mg, yield: 77%) as a yellow solid.

후처리

  1. extractionextracted with chloroform/methanol (9:1)
  2. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  3. concentrationconcentrated under reduced pressure
  4. customThe obtained residue was recrystallized from ethyl acetate

출처 및 근거

ORD 기록
ord-30bb5136152040fcac9317e2ba77789b
출처 데이터셋
uspto-grants-2012_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08232284B2

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