N-methyl-N-((R)-1-(methylcarbamoyl)-2-phenylethyl)carbamic acid tert-butyl ester → (R)-N-methyl-2-(methylamino)-3-phenylpropanamide

HRID 366175ノート

反応式

HRID 366175 の反応式
C(O[C:6](=O)[N:7](C)[C@@H:8]([C:16](=[O:19])[NH:17][CH3:18])[CH2:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)(C)(C)C>FC(F)(F)C(O)=O.C(Cl)Cl>[CH3:18][NH:17][C:16](=[O:19])[C@H:8]([NH:7][CH3:6])[CH2:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1

参加物

4

反応物 1

HCID 10613603N-methyl-N-((R)-1-(methylcarbamoyl)-2-phenylethyl)carbamic acid tert-butyl ester

生成物 1

HCID 10607786(R)-N-methyl-2-(methylamino)-3-phenylpropanamide収率 23.7%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 6422Trifluoroacetic acid溶媒

実験手順

N-Methyl-N-((R)1-(methylcarbamoyl)-2-phenylethyl)carbamic acid tert-butyl ester (1.39 g, 7.23 mmol) was dissolved in a mixture of trifluoroacetic acid (5 mL) and methylene chloride (10 mL) and stirred for 45 min. The volatiles were removed in vacuo and the residue was stirred with a mixture of ethyl acetate (100 mL) and water (100 mL). Sodium hydrogen carbonate (50 mL, saturated) was added and the phases were separated. The organic phase was dried (magnesium sulfate) and the solvent removed in vacuo to afford 330 mg of (R)-N-methyl-2-methylamino-3-phenylpropionamide.

後処理

  1. customThe volatiles were removed in vacuo
  2. stirringthe residue was stirred with a mixture of ethyl acetate (100 mL) and water (100 mL)
  3. additionSodium hydrogen carbonate (50 mL, saturated) was added
  4. customthe phases were separated
  5. dry with materialThe organic phase was dried (magnesium sulfate)
  6. customthe solvent removed in vacuo

出典と根拠

ORDレコード
ord-170b500465104c5a85afac87832079e3
出典データセット
uspto-grants-2000_10
特許番号
US06127391

反応ノート

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