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Cesium carbonate → {4-[3-(4-Chloro-2-phenoxy-phenoxy)-phenoxy]-2-methyl-phenylsulfanyl}-acetic acid

HRID 1822251
ノート
印刷プレビュー

反応式

HRID 1822251 の反応式
Br[C:2]1[CH:3]=[C:4]([CH:20]=[CH:21][CH:22]=1)[O:5][C:6]1[CH:11]=[CH:10][C:9]([Cl:12])=[CH:8][C:7]=1[O:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1.C([O:25][C:26](=[O:37])[CH2:27][S:28][C:29]1[CH:34]=[CH:33][C:32]([OH:35])=[CH:31][C:30]=1[CH3:36])C.CC(C)(C(=O)CC(=O)C(C)(C)C)C.C(=O)([O-])[O-].[Cs+].[Cs+].[OH-].[Na+]>CN1C(=O)CCC1.CO.[Cu]Cl>[Cl:12][C:9]1[CH:10]=[CH:11][C:6]([O:5][C:4]2[CH:3]=[C:2]([CH:22]=[CH:21][CH:20]=2)[O:35][C:32]2[CH:33]=[CH:34][C:29]([S:28][CH2:27][C:26]([OH:37])=[O:25])=[C:30]([CH3:36])[CH:31]=2)=[C:7]([O:13][C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[CH:8]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 5

HCID 10796Cesium carbonateHCID 14798Sodium HydroxideHCID 707002,2,6,6-Tetramethyl-3,5-heptanedioneHCID 578942271-(3-Bromo-phenoxy)-4-chloro-2-phenoxy-benzeneHCID 59164200(4-Hydroxy-2-methyl-phenylsulfanyl)-acetic acid ethyl ester

生成物 1

HCID 11785199
{4-[3-(4-Chloro-2-phenoxy-phenoxy)-phenoxy]-2-methyl-phenylsulfanyl}-acetic acid
収率 40%

試薬・触媒・溶媒 3

HCID 62652Cuprous chloride触媒HCID 887Methanol溶媒HCID 13387N-methyl-2-pyrrolidone溶媒

実験手順

A solution of 1-(3-bromo-phenoxy)-4-chloro-2-phenoxy-benzene (0.15 g, 0.4 mmol), (4-hydroxy-2-methyl-phenylsulfanyl)-acetic acid ethyl ester (99 mg, 0.44 mmol), copper(I) chloride (20 mg, 0.2 mmol), 2,2,6,6-tetramethyl-3,5-heptanedione (0.02 mL, 0.1 mmol), and cesium carbonate (156 mg, 0.48 mmol) in NMP (3 mL) is heated to 120° C. The reaction is stirred overnight and cooled to rt. The reaction is quenched with 1N aqueous HCl and extracted with ethyl ether. The organic is washed with brine, dried over sodium sulfate, and filtered. The solvent is removed to afford the crude ester intermediate. The intermediate is treated with 5N NaOH (0.4 mL, 2.2 mmol) in MeOH (5 mL) and heated to reflux. The reaction is stirred at reflux for 2 hours and then cooled. The reaction is quenched with 1N aqueous HCl to give pH=4. The aqueous layer is extracted with ethyl ether. The organic layer is washed with brine, dried over sodium sulfate, and filtered. The solvent is removed to afford the crude product. The crude is purified by prep HPLC to afford 78 mg (40%) of desired product. 1H NMR (400 MHz, CDCl3); MS (ES+) m/z mass calculated for C27H21ClO5S 492, found 493 and 495 (M+1 and M+3, 100%).

後処理

  1. customThe reaction is quenched with 1N aqueous HCl
  2. extractionextracted with ethyl ether
  3. washThe organic is washed with brine
  4. dry with materialdried over sodium sulfate
  5. filtrationfiltered
  6. customThe solvent is removed
  7. customto afford the crude ester intermediate
  8. temperatureheated to reflux
  9. stirringThe reaction is stirred
  10. temperatureat reflux for 2 hours
  11. temperaturecooled
  12. customThe reaction is quenched with 1N aqueous HCl
  13. customto give pH=4
  14. extractionThe aqueous layer is extracted with ethyl ether
  15. washThe organic layer is washed with brine
  16. dry with materialdried over sodium sulfate
  17. filtrationfiltered
  18. customThe solvent is removed
  19. customto afford the crude product
  20. customThe crude is purified by prep HPLC

出典と根拠

ORDレコード
ord-a6996c2bcfca4d48a9f36a3a5444bbfb
出典データセット
uspto-grants-2009_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07608639B2

反応ノート

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