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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
ノート
印刷プレビュー

反応式

HRID 333407 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 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

生成物 1

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

試薬・触媒・溶媒 3

HCID 6228Dimethylformamide溶媒HCID 6344Dichloromethane溶媒2 回HCID 8471Triethylamine溶媒

実験手順

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%.

後処理

  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)

出典と根拠

ORDレコード
ord-48a247cd79834bdc8bd6a791ceca3591
出典データセット
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08877968B2

反応ノート

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