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Trifluoroacetic acid → 3,5-Dichlorobenzyl 2-(2-aminoethyl)morpholine-4-carboxylate

HRID 1480381
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HRID 1480381 반응식
C(OC([NH:8][CH2:9][CH2:10][CH:11]1[O:16][CH2:15][CH2:14][N:13]([C:17]([O:19][CH2:20][C:21]2[CH:26]=[C:25]([Cl:27])[CH:24]=[C:23]([Cl:28])[CH:22]=2)=[O:18])[CH2:12]1)=O)(C)(C)C.FC(F)(F)C(O)=O>C(Cl)Cl>[NH2:8][CH2:9][CH2:10][CH:11]1[O:16][CH2:15][CH2:14][N:13]([C:17]([O:19][CH2:20][C:21]2[CH:26]=[C:25]([Cl:27])[CH:24]=[C:23]([Cl:28])[CH:22]=2)=[O:18])[CH2:12]1
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참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 867226343,5-Dichlorobenzyl 2-(2-((tert-butoxycarbonyl)amino)ethyl)morpholine-4-carboxylate

생성물 1

HCID 867226353,5-Dichlorobenzyl 2-(2-aminoethyl)morpholine-4-carboxylate

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A mixture comprising of 3,5-dichlorobenzyl 2-(2-((tert-butoxycarbonyl)amino)ethyl)morpholine-4-carboxylate (step 1)(500 mg, 1.154 mmol) and trifluoroacetic acid (3556 μl, 46.2 mmol) in DCM (3.8 ml) was stirred for 1 hour at room temperature. The resulting mixture was concentrated under reduced pressure and the crude product was diluted with EtOAc. The mixture was washed with sat. NaHCO3 and the organic portion was separated, dried over MgSO4, filtered and concentrated under reduced pressure to afford the title compound;

후처리

  1. concentrationThe resulting mixture was concentrated under reduced pressure
  2. additionthe crude product was diluted with EtOAc
  3. washThe mixture was washed with sat. NaHCO3
  4. customthe organic portion was separated
  5. dry with materialdried over MgSO4
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-5edabf7675c446e98a97320ff952a1c5
출처 데이터셋
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09409895B2

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