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1,2-Dichloroethane → (R)-carbamic acid 3-[4-(4-amino-phenyl)-piperazin-1-yl]-3-oxo-1-phenyl-propyl ester

HRID 44213
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HRID 44213 반응식
[OH:1][C@@H:2]([C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)[CH2:3][C:4]([OH:6])=O.[N+:13]([C:16]1[CH:21]=[CH:20][C:19]([N:22]2[CH2:27][CH2:26][NH:25][CH2:24][CH2:23]2)=[CH:18][CH:17]=1)([O-])=O.C(Cl)CCl.C1C=C[C:35]2[N:40](O)N=NC=2C=1.[OH-:42].[NH4+]>O1CCCC1.CO.[Pd].O.C(OCC)(=O)C>[NH2:13][C:16]1[CH:21]=[CH:20][C:19]([N:22]2[CH2:27][CH2:26][N:25]([C:4](=[O:6])[CH2:3][C@@H:2]([O:1][C:35](=[O:42])[NH2:40])[C:7]3[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=3)[CH2:24][CH2:23]2)=[CH:18][CH:17]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

11

반응물 5

HCID 111,2-DichloroethaneHCID 14923Ammonium HydroxideHCID 757711-HydroxybenzotriazoleHCID 804471-(4-Nitrophenyl)piperazineHCID 6950815(R)-3-hydroxy-3-phenylpropionic acid

생성물 1

HCID 58387062(R)-carbamic acid 3-[4-(4-amino-phenyl)-piperazin-1-yl]-3-oxo-1-phenyl-propyl ester

시약·촉매·용매 5

HCID 23938Palladium촉매HCID 887Methanol용매HCID 962Water용매HCID 8028Tetrahydrofuran용매2회HCID 8857Ethyl Acetate용매

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온도
25 °C

실험 절차

(R)-3-hydroxy-3-phenylpropionic acid (3.0 mmole) and 4-nitro phenylpiperazine (3 mmole) were dissolved in 20 mL of tetrahydrofuran at a room temperature, and EDC (6.0 mmole, 1-Ethyl-3-(3-dimethylaminopropyl)-carbodiimide) and HOBt (6 mmole, N-Hydroxybenzotriazole) were added dropwise to the mixture. Then, the resulting mixture was stirred at 25° C. for 5 hours. 20 mL of ethyl acetate was added three times to the mixture to extract an organic phase, and the prepared organic phase was dried over anhydrous magnesium sulfate (2 g), and filtered, and the resulting filtrate was concentrated under a reduced pressure, and purified with column chromatography (hexane:ethyl acetate=1:1). The resulting reaction product (1 mmol) was dissolved in methanol (20 mL), and subject to the reduction reaction at the presence of a palladium on charcoal (Pd/C) for 5 hours. The resulting reduction reaction product was concentrated under a reduced pressure to remove methanol, and extracted several times with ethyl acetate to separate an organic phase. The prepared organic phase was dried over anhydrous magnesium sulfate, and filtered, and the resulting filtrate was concentrated under a reduced pressure to obtain an intermediate reduced to an amino group (NH2). The intermediate reaction product prepared thus was dissolved in hydrofuran (10 mL), and 1,1′-carbodiimidazole (2 mmol) was added to the reaction product, and stirred at a room temperature for 1 hour. Then, excessive ammonium hydroxide was added to the resulting reaction mixture, and the reaction mixture was stirred at a room temperature for additional 2 hours. The resulting reaction mixture was diluted with water, and extracted several times with ethyl acetate to obtain an organic phase. The prepared organic phase was dried over magnesium sulfate, and concentrated under a reduced pressure. The resulting pellet was purified with column chromatography (hexane:ethyl acetate=1:1 to ethyl acetate) to obtain a title compound.

후처리

  1. extractionto extract an organic phase
  2. dry with materialthe prepared organic phase was dried over anhydrous magnesium sulfate (2 g)
  3. filtrationfiltered
  4. concentrationthe resulting filtrate was concentrated under a reduced pressure
  5. custompurified with column chromatography (hexane:ethyl acetate=1:1)
  6. customThe resulting reduction reaction product
  7. concentrationwas concentrated under a reduced pressure
  8. customto remove methanol
  9. extractionextracted several times with ethyl acetate
  10. customto separate an organic phase
  11. dry with materialThe prepared organic phase was dried over anhydrous magnesium sulfate
  12. filtrationfiltered
  13. concentrationthe resulting filtrate was concentrated under a reduced pressure
  14. customto obtain an intermediate
  15. customThe intermediate reaction product
  16. customprepared thus
  17. stirringstirred at a room temperature for 1 hour
  18. stirringthe reaction mixture was stirred at a room temperature for additional 2 hours
  19. customThe resulting reaction mixture
  20. extractionextracted several times with ethyl acetate
  21. customto obtain an organic phase
  22. dry with materialThe prepared organic phase was dried over magnesium sulfate
  23. concentrationconcentrated under a reduced pressure
  24. customThe resulting pellet was purified with column chromatography (hexane:ethyl acetate=1:1 to ethyl acetate)

출처 및 근거

ORD 기록
ord-65376d398ebb4d9f834333972fe72c6c
출처 데이터셋
uspto-grants-2013_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08541409B2

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