3-Amino-1-propanol → HCID 66773976、化合物

HRID 1644814

反応式

HRID 1644814 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 66773976HCID 66773976、化合物収率 95%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

反応条件

温度
45 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-40afdde3d9d34abb9f55f3d86697f01a
出典データセット
uspto-grants-2012_02
特許番号
US08124636B2

関連ノート

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