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1,2-Dichloroethane → 1-{1-[(S)-2-amino-3-(4-methoxy-phenyl)propionyl]-4-phenylpiperidin-4-yl}butan-1-one

HRID 333407
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HRID 333407 반응식
C([C@:18]([NH2:31])([CH2:22][C:23]1[CH:28]=[CH:27][C:26]([O:29][CH3:30])=[CH:25][CH:24]=1)[C:19]([OH:21])=O)(OCC1C2C(=CC=CC=2)C2C1=CC=CC=2)=O.C(Cl)CCl.C1C=CC2N(O)N=NC=2C=1.Cl.[C:47]1([C:53]2([C:59](=[O:63])[CH2:60][CH2:61][CH3:62])[CH2:58][CH2:57][NH:56][CH2:55][CH2:54]2)[CH:52]=[CH:51][CH:50]=[CH:49][CH:48]=1.C(=O)([O-])O.[Na+]>ClCCl.C(N(CC)CC)C.CN(C)C=O>[NH2:31][C@@H:18]([CH2:22][C:23]1[CH:24]=[CH:25][C:26]([O:29][CH3:30])=[CH:27][CH:28]=1)[C:19]([N:56]1[CH2:57][CH2:58][C:53]([C:59](=[O:63])[CH2:60][CH2:61][CH3:62])([C:47]2[CH:48]=[CH:49][CH:50]=[CH:51][CH:52]=2)[CH2:54][CH2:55]1)=[O:21]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 5

HCID 111,2-DichloroethaneHCID 757711-HydroxybenzotriazoleHCID 516892Sodium BicarbonateHCID 30149101-(4-Phenylpiperidin-4-yl)butan-1-one hydrochlorideHCID 66988467(S)-2-Fmoc-amino-3-(4-methoxy-phenyl)propionic acid

생성물 1

HCID 66987881
1-{1-[(S)-2-amino-3-(4-methoxy-phenyl)propionyl]-4-phenylpiperidin-4-yl}butan-1-one
수율 44.1%

시약·촉매·용매 3

HCID 6228Dimethylformamide용매HCID 6344Dichloromethane용매2회HCID 8471Triethylamine용매

실험 절차

To a solution containing 11.9 g (28.5 mmol) of (S)-2-Fmoc-amino-3-(4-methoxy-phenyl)propionic acid dissolved in 120 mL of dichloromethane and 10 mL of dimethylformamide are added 5.51 g (38.9 mmol) of EDC and 5.25 g (38.9 mmol) of HOBt. After stirring for 30 minutes at room temperature, a solution of 6.95 g (26.1 mmol) of 1-(4-phenylpiperidin-4-yl)-butan-1-one hydrochloride and 18 mL of triethylamine in 150 mL of dichloromethane is added. The reaction medium is stirred for 2 hours, and saturated aqueous sodium hydrogen carbonate solution is then added. The organic compounds are extracted with dichloromethane. The organic phase is dried over magnesium sulfate and then filtered, and the solvents are evaporated off. The crude product is chromatographed on silica gel (eluent: 9/1 dichloromethane/methanol). 4.7 g of 1-{1-[(S)-2-amino-3-(4-methoxyphenyl)-propionyl]-4-phenylpiperidin-4-yl}butan-1-one in the form of an orange oil are obtained in a yield of 44%.

후처리

  1. stirringThe reaction medium is stirred for 2 hours
  2. extractionThe organic compounds are extracted with dichloromethane
  3. dry with materialThe organic phase is dried over magnesium sulfate
  4. filtrationfiltered
  5. customthe solvents are evaporated off
  6. customThe crude product is chromatographed on silica gel (eluent: 9/1 dichloromethane/methanol)

출처 및 근거

ORD 기록
ord-48a247cd79834bdc8bd6a791ceca3591
출처 데이터셋
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08877968B2

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