3-Amino-1-propanol → HCID 66773976, 화합물

HRID 1644814

반응식

HRID 1644814 반응식
[CH3:1][O:2][C:3](=[O:13])[CH:4](Br)[C:5]1[CH:10]=[CH:9][C:8]([F:11])=[CH:7][CH:6]=1.C(=O)([O-])[O-].[K+].[K+].[NH2:20][CH2:21][CH2:22][CH2:23][OH:24]>C(Cl)(Cl)Cl>[CH3:1][O:2][C:3](=[O:13])[CH:4]([C:5]1[CH:10]=[CH:9][C:8]([F:11])=[CH:7][CH:6]=1)[NH:20][CH2:21][CH2:22][CH2:23][OH:24]

참가 물질

5

반응물 3

HCID 90863-Amino-1-propanolHCID 11430Potassium CarbonateHCID 12717580Methyl 2-bromo-2-(4-fluorophenyl)acetate

생성물 1

HCID 66773976HCID 66773976, 화합물수율 95%

시약·촉매·용매 1

HCID 6212Chloroform용매

반응 조건

온도
45 °C

실험 절차

To a solution of bromo-(4-fluoro-phenyl)-acetic acid methyl ester (16.0 g) in chloroform (100 mL) was added potassium carbonate (17.9 g, finely ground) followed by 3-amino-1-propanol (4.87 g). The reaction was heated to 45° C. for 18 hours. The reaction was filtered and the filtrate was diluted with water and the phases were separated. The aqueous phase was further extracted with chloroform (3×25 mL) and the combined organics were washed with brine. The chloroform phase was dried over sodium sulfate, filtered and evaporated in vacuo to give the desired (4-fluoro-phenyl)-(3-hydroxy-propylamino)-acetic acid methyl ester (14.85 g, MS (ES+): 242.2 (MH+)) as a yellow oil which was used in the next step without further purification.

후처리

  1. filtrationThe reaction was filtered
  2. additionthe filtrate was diluted with water
  3. customthe phases were separated
  4. extractionThe aqueous phase was further extracted with chloroform (3×25 mL)
  5. washthe combined organics were washed with brine
  6. dry with materialThe chloroform phase was dried over sodium sulfate
  7. filtrationfiltered
  8. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-40afdde3d9d34abb9f55f3d86697f01a
출처 데이터셋
uspto-grants-2012_02
특허 번호
US08124636B2

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