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Triethylamine → 1-[2-(2,4-Dibenzyloxyphenylacetyl)aminoethyl]piperidine

HRID 981413
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HRID 981413 반응식
[NH2:1][CH2:2][CH2:3][N:4]1[CH2:9][CH2:8][CH2:7][CH2:6][CH2:5]1.[CH2:10]([O:17][C:18]1[CH:23]=[C:22]([O:24][CH2:25][C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)[CH:21]=[CH:20][C:19]=1[CH2:32][C:33](O)=[O:34])[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.C(N(CC)CC)C.C(OP(C#N)(OCC)=O)C>CN(C)C=O.O>[CH2:10]([O:17][C:18]1[CH:23]=[C:22]([O:24][CH2:25][C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)[CH:21]=[CH:20][C:19]=1[CH2:32][C:33]([NH:1][CH2:2][CH2:3][N:4]1[CH2:9][CH2:8][CH2:7][CH2:6][CH2:5]1)=[O:34])[C:11]1[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 8471TriethylamineHCID 33944N-(2-Aminoethyl)piperidineHCID 76257Diethyl cyanophosphonateHCID 50283782-[2,4-Bis(benzyloxy)phenyl]acetic Acid

생성물 1

HCID 200715791-[2-(2,4-Dibenzyloxyphenylacetyl)aminoethyl]piperidine수율 72.2%

시약·촉매·용매 2

HCID 962
Water
용매
HCID 6228Dimethylformamide용매

실험 절차

To a solution of 1-(2-aminoethyl)piperidine (368 mg) and 2,4-dibenzyloxyphenylacetic acid (1.0 g) in N,N-dimethylformamide are added triethylamine (1.2 ml) and diethylcyanophosphate (561 mg) in sequence. The mixture is stirred at room temperature for 30 minutes. To the reaction solution is added water and stirring carried out for 10 minutes. The product is extracted with dichloromethane. The dichloromethane layer is washed with water and dried over anhydrous sodium sulfate. The solvent is distilled off and the residue obtained is purified by silica gel column chromatography. The fractions eluted with dichloro-methane-methanol mixture (10 : 1) is recrystallized from dichloromethane-n-hexane mixture (1 : 5) to obtain 1-[2-(2,4-dibenzyloxyphenylacetyl)aminoethyl]piperidine (950 mg) in the colorless needle-like crystal form.

후처리

  1. stirringstirring
  2. waitcarried out for 10 minutes
  3. extractionThe product is extracted with dichloromethane
  4. washThe dichloromethane layer is washed with water
  5. dry with materialdried over anhydrous sodium sulfate
  6. distillationThe solvent is distilled off
  7. customthe residue obtained
  8. customis purified by silica gel column chromatography
  9. washThe fractions eluted with dichloro-methane-methanol mixture (10 : 1)
  10. customis recrystallized from dichloromethane-n-hexane mixture (1 : 5)

출처 및 근거

ORD 기록
ord-cadab5d6c7464fca9fbed4fd10b6da8d
출처 데이터셋
uspto-grants-1991_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04990511

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