Hydrochloric Acid → Methyl phenethylcarbamate

HRID 1593

反応式

HRID 1593 の反応式
[CH2:1]([NH2:9])[CH2:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.C(N(CC)CC)C.Cl[C:18]([O:20][CH3:21])=[O:19].Cl>C1COCC1.C(OCC)C>[CH3:21][O:20][C:18]([NH:9][CH2:1][CH2:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1)=[O:19]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 1001PhenethylamineHCID 6586Methyl chloroformateHCID 8471Triethylamine

生成物 1

HCID 4380476Methyl phenethylcarbamate収率 95%

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a stirred solution of phenethylamine (75.2 mL, 0.6 mol) and triethylamine (83 mL, 0.6 mol) in THF (500 mL) was added slowly methyl chloroformate 46.2 mL, 0.6 mol) dissolved in THF (50 mL). After the reaction was stirred for an additional 1 h at room temperature, diethyl ether (2 L) and 1N HCl (800 mL) were added. The organic layer was washed with water, dried (MgSO4), filtered, and the filtrate was concentrated in vacuo to give a clear oil of pure title compound (102 g, 95%).

後処理

  1. washThe organic layer was washed with water
  2. dry with materialdried (MgSO4)
  3. filtrationfiltered
  4. concentrationthe filtrate was concentrated in vacuo

出典と根拠

ORDレコード
ord-bbd17ea5df144cd0a50c633bd92af129
出典データセット
uspto-grants-1998_03
特許番号
US05726159

関連ノート

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