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Dichloromethane → Ethyl 2-(benzylamino)acetate Hydrochloride

HRID 1588248
ノート
印刷プレビュー

反応式

HRID 1588248 の反応式
[CH2:1]([NH2:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(N(CC)CC)C.Br[CH2:17][C:18]([O:20][CH2:21][CH3:22])=[O:19].C(Cl)[Cl:24]>>[ClH:24].[CH2:21]([O:20][C:18](=[O:19])[CH2:17][NH:8][CH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1)[CH3:22]
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 4

HCID 6344DichloromethaneHCID 7504BenzylamineHCID 7748Ethyl bromoacetateHCID 8471Triethylamine

生成物 1

HCID 2724714Ethyl 2-(benzylamino)acetate Hydrochloride収率 28%

実験手順

In a 3 liter erlenmeyer flask was placed 107.2 g (1.0 mole) of benzylamine, 152.0 g (1.5 mole) of triethylamine and 1.5 liter of methylene chloride. The resulting solution was stirred while 167.0 g (1.0 mole) of ethyl bromoacetate was added dropwise. The mixture was washed with water (3×300 mL), dried over magnesium sulfate, filtered and solvent was removed by rotary evaporation. The resulting oil was dissolved in ether and hydrogen chloride saturated ether was then added slowly until precipitation was complete. The precipitate was a gummy solid and the mixture was stoppered and let sit for one day. Over this time the precipitate formed a hard solid which was filtered off and dried in vacuum to give 62.8 g (28%) of N-benzylglycine ethyl ester hydrochloride.

後処理

  1. customIn a 3 liter erlenmeyer flask was placed
  2. additionwas added dropwise
  3. washThe mixture was washed with water (3×300 mL)
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered
  6. customsolvent was removed by rotary evaporation
  7. dissolutionThe resulting oil was dissolved in ether
  8. additionhydrogen chloride saturated ether was then added slowly until precipitation
  9. customOver this time the precipitate formed a hard solid which
  10. filtrationwas filtered off
  11. customdried in vacuum

出典と根拠

ORDレコード
ord-2dc907d7d0c74193b27e18ef73470e44
出典データセット
uspto-grants-1993_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05221665

反応ノート

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