3-Hydroxybenzaldehyde → 2-(3-formylphenoxy)acetamide

HRID 639726노트

반응식

HRID 639726 반응식
[OH:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][CH:9]=1)[CH:5]=[O:6].Cl[CH2:11][C:12]([NH2:14])=[O:13].C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[NH2:14][C:12]([CH2:11][O:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][CH:9]=1)[CH:5]=[O:6])=[O:13]

참가 물질

5

반응물 3

HCID 1013-HydroxybenzaldehydeHCID 6580ChloroacetamideHCID 11430Potassium Carbonate

생성물 1

HCID 110844662-(3-formylphenoxy)acetamide수율 72.8%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
90 °C

실험 절차

To a mixture of 12.21 g of 3-hydroxybenzaldehyde, 14.00 g of 2-chloroacetamide and 60 ml of dimethylformamide was added 20.70 g of potassium carbonate, and this was heated to stir at 90° C. for 2 hours. After cooled to room temperature, insolubles were filtered and the filtrate was concentrated under reduced pressure. The resulting residue was dissolved in tetrahydrofuran by heating. Insolubles were filtered and the filtrate was concentration under reduced pressure. The resulting crude crystals were washed with a mixed solution of tetrahydrofuran and t-butyl methyl ether and dried to obtain 13.05 g of 3-(aminocarbonylmethoxy)benzaldehyde [Compound No. (n)] as a crystal.

후처리

  1. temperaturethis was heated
  2. temperatureAfter cooled to room temperature
  3. filtrationinsolubles were filtered
  4. concentrationthe filtrate was concentrated under reduced pressure
  5. dissolutionThe resulting residue was dissolved in tetrahydrofuran
  6. temperatureby heating
  7. filtrationInsolubles were filtered
  8. concentrationconcentration under reduced pressure
  9. washThe resulting crude crystals were washed with a mixed solution of tetrahydrofuran and t-butyl methyl ether
  10. customdried

출처 및 근거

ORD 기록
ord-6644c46d1a3542499f32cf5648ae6866
출처 데이터셋
uspto-grants-2010_04
특허 번호
US07691883B2

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