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Citric Acid → (4-Chloro-3-{(1e)-3-[2-(4-methylbenzoyl)-1h-pyrrol-1-yl]-1-propenyl}phenoxy)acetic acid

HRID 1352861
ノート
印刷プレビュー

反応式

HRID 1352861 の反応式
Cl[C:2]1[CH:16]=[CH:15][C:14](/[CH:17]=[CH:18]/[CH2:19]O)=[CH:13][C:3]=1[O:4][CH2:5][C:6]([O:8]C(C)(C)C)=[O:7].C([N:23]([CH2:26][CH3:27])[CH2:24][CH3:25])C.CS([Cl:32])(=O)=O.[C:33](O)(=O)[CH2:34][C:35]([CH2:40][C:41](O)=O)([C:37]([OH:39])=O)O.[Br-].[Li+].C[C:49]([CH3:52])([O-])C.[K+].[OH-].[Na+]>O1CCCC1.CO.O>[Cl:32][C:15]1[CH:16]=[CH:2][C:3]([O:4][CH2:5][C:6]([OH:8])=[O:7])=[CH:13][C:14]=1/[CH:17]=[CH:18]/[CH2:19][N:23]1[CH:24]=[CH:25][CH:27]=[C:26]1[C:37](=[O:39])[C:35]1[CH:34]=[CH:33][C:49]([CH3:52])=[CH:41][CH:40]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

11

反応物 7

HCID 311Citric AcidHCID 8471TriethylamineHCID 14798Sodium HydroxideHCID 31297Methanesulfonyl chlorideHCID 82050Lithium BromideHCID 23665647Potassium tert-butoxideHCID 131726453t-Butyl {2-chloro-5-[(1e)-3-hydroxy-1-propenyl]phenoxy}acetate

生成物

1
HCID 22928718(4-Chloro-3-{(1e)-3-[2-(4-methylbenzoyl)-1h-pyrrol-1-yl]-1-propenyl}phenoxy)acetic acid収率 29%

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a solution of the compound of Example 20-4 in tetrahydrofuran (5.0 ml) were added under ice cooling triethylamine (0.270 ml, 1.94 mmol) and methanesulfonyl chloride (0.110 ml, 1.42 mmol) in the order. The mixture was stirred for 1 hour under ice cooling. To the reaction mixture were added cold 10% aqueous citric acid solution and the mixture was extracted with ethyl acetate. The organic layer was washed with cold 10% aqueous citric acid solution and a cold aqueous saturated sodium hydrogencarbonate solution in the order and dried over sodium sulfate. The solvent was removed and the residue was dissolve in tetrahydrofuran (2.0 ml). Thereto was added lithium bromide (2.61 mg, 3.00 mmol) and the mixture was stirred for 3 hours. To the reaction mixture was added water and extracted with ethyl acetate. The organic layer was washed with water and an aqueous saturated sodium chloride solution and dried over sodium sulfate. The solvent was removed and the residue was dissolved in tetrahydrofuran (2 ml). The solution was dropped into a solution of the compound (185 mg, 1.00 mmol) of Reference example 1 and potassium t-butoxide (112 mg, 1.00 mmol) in tetrahydrofuran (2 ml) under ice cooling. The mixture was stirred for 5 hours under ice cooling. Thereto were added methanol (2.0 ml) and an aqueous 1N sodium hydroxide solution (2.0 ml) and the mixture was stirred for 2 hours at room temperature. The reaction mixture was washed with hexane and ether and acidified with potassium hydrogensulfate. The mixture was extracted with chloroform and the organic layer was washed with an aqueous saturated sodium chloride solution and dried over sodium sulfate. The solvent was removed and purified with silica gel chromatography (chloroform:methanol, 10:1) to give the subject compound (177 mg, 29%).

後処理

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe organic layer was washed with cold 10% aqueous citric acid solution
  3. dry with materiala cold aqueous saturated sodium hydrogencarbonate solution in the order and dried over sodium sulfate
  4. customThe solvent was removed
  5. dissolutionthe residue was dissolve in tetrahydrofuran (2.0 ml)
  6. stirringthe mixture was stirred for 3 hours
  7. extractionextracted with ethyl acetate
  8. washThe organic layer was washed with water
  9. dry with materialan aqueous saturated sodium chloride solution and dried over sodium sulfate
  10. customThe solvent was removed
  11. dissolutionthe residue was dissolved in tetrahydrofuran (2 ml)
  12. stirringThe mixture was stirred for 5 hours under ice cooling
  13. washThe reaction mixture was washed with hexane and ether
  14. extractionThe mixture was extracted with chloroform
  15. washthe organic layer was washed with an aqueous saturated sodium chloride solution
  16. dry with materialdried over sodium sulfate
  17. customThe solvent was removed
  18. custompurified with silica gel chromatography (chloroform:methanol, 10:1)

出典と根拠

ORDレコード
ord-30a52c10d90e4491b6292e33767c4360
出典データセット
uspto-grants-2007_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07220773B2

反応ノート

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