Sodium Iodide → 4-Methoxycarbonylmethoxy-benzoic acid [1-methoxycarbonyl-2-(4-methoxy carbonyl methoxy-phenyl)-ethylcarbamoyl]-methoxycarbonylmethyl ester

HRID 546364ノート

反応式

HRID 546364 の反応式
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][CH:9]([NH:14][C:15]([CH:17]([O:22][C:23](=[O:31])[C:24]2[CH:29]=[CH:28][C:27]([OH:30])=[CH:26][CH:25]=2)[C:18]([O:20][CH3:21])=[O:19])=[O:16])[C:10]([O:12][CH3:13])=[O:11])=[CH:4][CH:3]=1.[I-].[Na+].P(O)([O-])([O-])=O.[Na+].[Na+]>CC(C)=O>[CH3:13][O:12][C:10]([CH:9]([NH:14][C:15]([CH:17]([O:22][C:23](=[O:31])[C:24]1[CH:25]=[CH:26][C:27]([O:30][CH2:17][C:18]([O:20][CH3:21])=[O:19])=[CH:28][CH:29]=1)[C:18]([O:20][CH3:21])=[O:19])=[O:16])[CH2:8][C:5]1[CH:6]=[CH:7][C:2]([O:1][CH2:9][C:10]([O:12][CH3:13])=[O:11])=[CH:3][CH:4]=1)=[O:11]

参加物

5

反応物 3

HCID 5238Sodium IodideHCID 24203Sodium Phosphate, DibasicHCID 671882054-Hydroxy-benzoic acid [2-(4-hydroxy-phenyl)-1-methoxycarbonyl-ethyl carbamoyl]-methoxycarbonylmethyl ester

生成物 1

HCID 671894534-Methoxycarbonylmethoxy-benzoic acid [1-methoxycarbonyl-2-(4-methoxy carbonyl methoxy-phenyl)-ethylcarbamoyl]-methoxycarbonylmethyl ester

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

To a mixture of 4-hydroxy-benzoic acid [2-(4-hydroxy-phenyl)-1-methoxycarbonyl-ethyl carbamoyl]-methoxycarbonylmethyl ester 17 (10.7 grams, 24.82 mmol) anhydrous potassium carbonate (17.5 grams, 126.62 mmol), sodium iodide (3 grams, 20.01 mmol), and disodium phosphate (3 grams, 21.13 mmol) in anhydrous acetone (100 mL) is added methyl chloro acetate (7 grams, 64.5 mmol). The mixture is refluxed for 10 hours. Acetone is distilled off, and water (100 mL) is added. Crude 18 is filtered, dried, and can be purified in appropriate solvent.

後処理

  1. temperatureThe mixture is refluxed for 10 hours
  2. distillationAcetone is distilled off
  3. additionwater (100 mL) is added
  4. filtrationCrude 18 is filtered
  5. customdried
  6. customcan be purified in appropriate solvent

出典と根拠

ORDレコード
ord-2973e85d6fc043888793a10857ed1a82
出典データセット
uspto-grants-2011_05
特許番号
US07935843B2

反応ノート

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