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Potassium Carbonate → 2-([(Benzyloxy)carbonyl]amino)-3-methoxypropanoic acid

HRID 965201
ノート
印刷プレビュー

反応式

HRID 965201 の反応式
C[O:2][C:3](=[O:19])[CH:4]([NH:8][C:9]([O:11][CH2:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)=[O:10])[CH2:5][O:6][CH3:7].C([O-])([O-])=O.[K+].[K+]>CO>[C:9]([NH:8][CH:4]([CH2:5][O:6][CH3:7])[C:3]([OH:19])=[O:2])([O:11][CH2:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)=[O:10]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 11430Potassium CarbonateHCID 12344754Methyl 2-(((benzyloxy)carbonyl)amino)-3-methoxypropanoate

生成物 1

HCID 123447572-([(Benzyloxy)carbonyl]amino)-3-methoxypropanoic acid収率 95%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Compound 10 (0.58 g) was dissolved in 80% aqueous methanol (3.0 mL). To this solution was added anhydrous K2CO3 (0.5 g) and the reaction mixture was stirred at room temperature (8 hours). The methanol was evaporated in vacuo and the residue suspended in water (50 mL). The aqueous suspension was washed with ethyl ether (2×25 mL) and then acidified to pH 3.0 using 5N HCl. The acidified aqueous phase was extracted with ethyl acetate (3×25 mL). The ethyl acetate extracts were combined, dried (Na2SO4), filtered, and evaporated in vacuo to obtain pure 11 as a clear viscous oil (0.52 g, 95%): Rf 0.30 (10% MeOH/CHCl3).

後処理

  1. customThe methanol was evaporated in vacuo
  2. washThe aqueous suspension was washed with ethyl ether (2×25 mL)
  3. extractionThe acidified aqueous phase was extracted with ethyl acetate (3×25 mL)
  4. dry with materialdried (Na2SO4)
  5. filtrationfiltered
  6. customevaporated in vacuo

出典と根拠

ORDレコード
ord-1940224b0efb48f18c4dde024ccc61d7
出典データセット
uspto-grants-1998_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05773475

反応ノート

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