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Methanol → 2-[(6-Methoxypyrazin-2-ylamino)methyl]phenol

HRID 2170003
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HRID 2170003 반응식
Br[C:2]1[N:7]=[C:6]([NH:8][CH2:9][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=2[OH:16])[CH:5]=[N:4][CH:3]=1.[CH3:17][OH:18].[OH-].[Na+].[Cl-].[NH4+]>C(OCC)(=O)C>[CH3:17][O:18][C:2]1[N:7]=[C:6]([NH:8][CH2:9][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=2[OH:16])[CH:5]=[N:4][CH:3]=1
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참가 물질

6

반응물 4

HCID 887MethanolHCID 14798Sodium HydroxideHCID 25517Ammonium ChlorideHCID 53250722HCID 53250722, 화합물

생성물 1

HCID 532507282-[(6-Methoxypyrazin-2-ylamino)methyl]phenol

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

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온도
150 °C

실험 절차

Introduced into a microwave tube are 363 mg (1.29 mmol) of 2-[(6-bromopyrazin-2-ylamino)methyl]phenol, prepared as described previously in Example 12, to which 3 ml of methanol and 103 mg (2.58 mmol, 2 eq) of sodium hydroxide are added. The reaction mixture is then heated for 30 mins in a microwave oven at 150° C. and is then diluted with 50 ml of ethyl acetate. The mixture is neutralized with an ammonium chloride solution to pH=7, decanted and the organic phase is washed twice with 50 ml of water. The organic phase is dried over magnesium sulphate, filtered, and concentrated to dryness. The residue is purified by chromatography over silica with, as eluent, heptane/ethyl acetate (7/3). 2-[(6-Methoxypyrazin-2-ylamino)methyl]phenol is obtained in the form of a white solid.

후처리

  1. additionIntroduced into a microwave tube
  2. customprepared
  3. additionare added
  4. customdecanted
  5. washthe organic phase is washed twice with 50 ml of water
  6. dry with materialThe organic phase is dried over magnesium sulphate
  7. filtrationfiltered
  8. concentrationconcentrated to dryness
  9. customThe residue is purified by chromatography over silica with, as eluent

출처 및 근거

ORD 기록
ord-23203c035d7f4028b25166ce670367ae
출처 데이터셋
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09050266B2

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