Trifluoroacetic acid → (Benzyloxy)(ethyl)amine

HRID 2403235ノート

反応式

HRID 2403235 の反応式
[CH2:1]([O:8][N:9]([CH2:17][CH3:18])C(=O)OC(C)(C)C)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(O)(C(F)(F)F)=O>C(Cl)Cl>[CH2:1]([O:8][NH:9][CH2:17][CH3:18])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 86675732Tert-butyl benzyloxy(ethyl)carbamate

生成物 1

HCID 251744(Benzyloxy)(ethyl)amine収率 88%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

151 (616 mg) was dissolved in 4 ml of DCM and 4 ml of TFA was added then the reaction mixture was let 1 h at room temperature. The reaction mixture is concentrated and 50 ml of AcOEt are added. The organic phase are washed with saturated NaHCO3 and brine then dried over Na2SO4, filtered and concentrated to afford 152 as an oil (324 mg, 88%). 1H NMR (DMSO): δ 0.99 (t, 3H, J=7.3 Hz), 2.82 (m, 2H), 4.61 (s, 2H), 6.50 (t, 1H, J=5.8 Hz), 7.32 (m, 5H).

後処理

  1. concentrationThe reaction mixture is concentrated
  2. addition50 ml of AcOEt are added
  3. washThe organic phase are washed with saturated NaHCO3 and brine
  4. dry with materialthen dried over Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-5294eab2452c486386a305cdfad73fe4
出典データセット
uspto-grants-2014_08
特許番号
US08802666B2

反応ノート

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