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Sodium Hydroxide → 2-(2-Fluoro-phenoxy)-3-(4-hydroxy-phenyl)-2-methyl-propionic acid methylester

HRID 1985125
ノート
印刷プレビュー

反応式

HRID 1985125 の反応式
[Li+].CC([N-]C(C)C)C.[CH2:9]([O:11][C:12](=[O:23])[CH:13]([O:15][C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=1[F:22])[CH3:14])C.I[CH2:25][C:26]1[CH:31]=[CH:30][C:29]([O:32]S(C2C=CC(C)=CC=2)(=O)=O)=[CH:28][CH:27]=1.[OH-].[Na+]>C1COCC1.CO>[CH3:9][O:11][C:12](=[O:23])[C:13]([O:15][C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=1[F:22])([CH3:14])[CH2:25][C:26]1[CH:27]=[CH:28][C:29]([OH:32])=[CH:30][CH:31]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 14798Sodium HydroxideHCID 2724682Lithium diisopropylamideHCID 57719284Ethyl 2-(2-fluorophenoxy)propanoateHCID 86596228Toluene-4-sulfonic acid 4-iodomethyl-phenyl ester

生成物 1

HCID 688682502-(2-Fluoro-phenoxy)-3-(4-hydroxy-phenyl)-2-methyl-propionic acid methylester収率 60%

試薬・触媒・溶媒 2

HCID 887
Methanol
溶媒
HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
-78 °C

実験手順

To a solution of LDA (1.5 M in cyclohexane, 33 mL, 49.5 mmole) in THF (40 mL), at −78° C., is added dropwise a solution of 2-(2-fluoro-phenoxy)-propionic acid ethyl ester (7.70 g, 36.3 mmole) in THF (100 mL). After stirring for 30 minutes at −78° C., a solution of toluene-4-sulfonic acid 4-iodomethyl-phenyl ester (12.8 g, 33.0 mmole) is injected to the reaction mixture. The reaction is stirred at −78° C. for one hour, then warmed up to room temperature and stirred overnight. The reaction is treated with 5.0N NaOH (50 mL) in presence of methanol (200 mL). After evaporating methanol, the aqueous solution is acidified with concentrated HCl to pH=1 and is extracted with ethyl acetate (2×300 mL). The combined organic layers are dried, filtered and concentrated in vacuo. The residue is dissolved in MeOH (200 mL) and treated with concentrated sulfuric acid (2 mL) at 80° C. overnight. The reaction mixture is partitioned between ethyl acetate (500 mL) and water (500 mL), the organic layer is washed by brine (3×500 mL), dried, filtered and concentrated in vacuo. The compound is purified by chromatography (silica gel, gradient elution 0-20% ethyl acetate in hexane) to provide an oil (6.02 g, 60%), which is then resolved by chiral HPLC to generate the enantiomer as an oil (2.30 g). Mass [EI+] 322 (M+NH4)+, [EI−] 303 (M−H)−.

後処理

  1. stirringThe reaction is stirred at −78° C. for one hour
  2. temperaturewarmed up to room temperature
  3. stirringstirred overnight
  4. customAfter evaporating methanol
  5. extractionis extracted with ethyl acetate (2×300 mL)
  6. customThe combined organic layers are dried
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo
  9. dissolutionThe residue is dissolved in MeOH (200 mL)
  10. additiontreated with concentrated sulfuric acid (2 mL) at 80° C. overnight
  11. customThe reaction mixture is partitioned between ethyl acetate (500 mL) and water (500 mL)
  12. washthe organic layer is washed by brine (3×500 mL)
  13. customdried
  14. filtrationfiltered
  15. concentrationconcentrated in vacuo
  16. customThe compound is purified by chromatography (silica gel, gradient elution 0-20% ethyl acetate in hexane)

出典と根拠

ORDレコード
ord-4fa916bf465a40a28cfcff50fff5a305
出典データセット
uspto-grants-2009_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07544812B2

反応ノート

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