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Triethylamine → N-[(4-Fluorophenyl)sulfonyl]-D-aspartic Acid 1,4-Dimethyl Ester

HRID 1036628
ノート
印刷プレビュー

反応式

HRID 1036628 の反応式
Cl.[CH3:2][O:3][C:4](=[O:12])[C@@H:5]([CH2:7][C:8]([O:10][CH3:11])=[O:9])[NH2:6].[F:13][C:14]1[CH:19]=[CH:18][C:17]([S:20](Cl)(=[O:22])=[O:21])=[CH:16][CH:15]=1.C(N(CC)CC)C>C1COCC1>[F:13][C:14]1[CH:19]=[CH:18][C:17]([S:20]([NH:6][C@@H:5]([C:4]([O:3][CH3:2])=[O:12])[CH2:7][C:8]([O:10][CH3:11])=[O:9])(=[O:22])=[O:21])=[CH:16][CH:15]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8471TriethylamineHCID 95884-Fluorobenzenesulfonyl chlorideHCID 510515941,4-dimethyl (2R)-2-aminobutanedioate hydrochloride

生成物 1

HCID 36586805N-[(4-Fluorophenyl)sulfonyl]-D-aspartic Acid 1,4-Dimethyl Ester収率 86%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a suspension of D-aspartic acid dimethyl ester hydrochloride (36.0 g, 182 mmol) in THF (360 mL) was added 4-fluorobenzenesulfonyl chloride (39.0 g, 200 mmol, 1.1 equiv.). To the previous mixture at 0° C. was added dropwise triethylamine (60.8 g, 601 mmol, 3.3 equiv.). After a period of 18 h at room temperature, the reaction mixture was filtered and the solid washed with methyl tert-butyl ether (30 mL). The filtrate was evaporated followed by the addition of methyl tert-butyl ether (300 mL). To the resulting mixture was added 100 mL of HCl 1 M. The organic phase was separated and sequentially washed with water, half-saturated sodium bicarbonate, HCl 0.5 M and half-saturated sodium chloride. The organic phase was dried over magnesium sulfate, filtered and evaporated under reduced pressure to give 50 g of the title compound as an oil.

後処理

  1. filtrationthe reaction mixture was filtered
  2. washthe solid washed with methyl tert-butyl ether (30 mL)
  3. customThe filtrate was evaporated
  4. additionfollowed by the addition of methyl tert-butyl ether (300 mL)
  5. additionTo the resulting mixture was added 100 mL of HCl 1 M
  6. customThe organic phase was separated
  7. washsequentially washed with water, half-saturated sodium bicarbonate, HCl 0.5 M and half-saturated sodium chloride
  8. dry with materialThe organic phase was dried over magnesium sulfate
  9. filtrationfiltered
  10. customevaporated under reduced pressure

出典と根拠

ORDレコード
ord-1eb503b1ad414b5fa8c1c8228b8f9971
出典データセット
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08546422B2

反応ノート

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