Triethylamine → HCID 40493097, 화합물

HRID 1842707노트

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HRID 1842707 반응식
Br[CH2:2][C:3]([O:5][CH3:6])=[O:4].[C:7]1([C@H:13]([NH2:15])[CH3:14])[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.C(N(CC)CC)C>CCOC(C)=O>[C:7]1([C@H:13]([NH:15][CH2:2][C:3]([O:5][CH3:6])=[O:4])[CH3:14])[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 60984Methyl bromoacetateHCID 6431891-Phenethylamine, (+)-

생성물 1

HCID 40493097HCID 40493097, 화합물수율 90%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

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온도
55 °C

실험 절차

Methyl 2-bromoacetate (621 g, 4.1 mol) was added dropwise to a mixture of (1R)-1-phenylethanamine (410 g, 3.4 mol) and triethylamine (377 g, 3.7 mol) in EtOAc (4.5 L) at r.t. The mixture was then stirred at 50-60° C. overnight then cooled to r.t. The mixture was then washed with water (800 mL) and brine (100 mL), dried (Na2SO4) and concentrated in vacuo to give the title compound (587 g, 90%) as yellow oil; 1H NMR: (CDCl3) 1.29 (3H, d), 3.13-3.24 (2H, m), 3.60 (3H, s), 3.68-3.71 (1H, m), 7.13-7.26 (5H, m).

후처리

  1. temperaturethen cooled to r.t
  2. washThe mixture was then washed with water (800 mL) and brine (100 mL)
  3. dry with materialdried (Na2SO4)
  4. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-51a8c7e831a942c7b2d7873ef204d84a
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08946235B2

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