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1,2-Dichloroethane → HCID 59511790, Verbindung

HRID 1157449
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1157449
Cl.Cl.[NH2:3][C:4]1[CH:12]=[CH:11][C:10]([O:13][CH2:14][CH2:15][CH2:16][N:17]2[CH2:22][CH2:21][CH2:20][CH2:19][CH2:18]2)=[CH:9][C:5]=1[C:6]([OH:8])=[O:7].[NH2:23][CH2:24][C:25]([NH:27][CH:28]([CH3:30])[CH3:29])=[O:26].C(N(CC)CC)C.C(Cl)CCl.C1C=CC2N(O)N=NC=2C=1>CN(C=O)C.CO>[NH4+:3].[OH-:7].[NH2:3][C:4]1[CH:12]=[CH:11][C:10]([O:13][CH2:14][CH2:15][CH2:16][N:17]2[CH2:22][CH2:21][CH2:20][CH2:19][CH2:18]2)=[CH:9][C:5]=1[C:6]([NH:23][CH2:24][C:25](=[O:26])[NH:27][CH:28]([CH3:30])[CH3:29])=[O:8]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

9

Edukt 5

HCID 111,2-DichloroethaneHCID 8471TriethylamineHCID 757711-HydroxybenzotriazoleHCID 5338492-Amino-N-isopropylacetamideHCID 68521714HCID 68521714, Verbindung

Produkt 2

HCID 14923Ammonium Hydroxide
HCID 59511790
HCID 59511790, Verbindung
Ausbeute 200 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

A mixture of 2-amino-5-(3-piperidin-1-ylpropoxy)benzoic acid dihydrochloride (1.3 g, 3.7 mmol), 2-amino-N-isopropylacetamide*HCl (INTERMEDIATE I.1) (557 mg, 3.7 mmol) and triethylamine (2.1 mL, 14.8 mmol) in DMF (20 mL) was stirred at room temperature for 10 min. EDC (851 mg, 4.4 mmol) and HOBt (600 mg, 4.4 mmol) were added and stirring continued at room temperature for 16 h. The mixture was partitioned between ethyl acetate (100 mL) and 2N Na2CO3 (aq.) (100 mL) and the aqueous extracted with additional ethyl acetate (2×100 mL). The combined organics were washed with brine (1×100 mL), dried (MgSO4), filtered and concentrated in vacuo. The crude residue was purified by chromatography on silica gel with dichloromethane:methanol: NH4OH (aq.) (160:39:1, v/v) as eluent to provide 2-amino-N-(isopropylcarbamoylmethyl)-5-(3-piperidin-1-ylpropoxy)benzamide (INTERMEDIATE V1.1) (1.4 g, 3.7 mmol, 100%).

Aufarbeitung

  1. stirringstirring
  2. waitcontinued at room temperature for 16 h
  3. customThe mixture was partitioned between ethyl acetate (100 mL) and 2N Na2CO3 (aq.) (100 mL)
  4. extractionthe aqueous extracted with additional ethyl acetate (2×100 mL)
  5. washThe combined organics were washed with brine (1×100 mL)
  6. dry with materialdried (MgSO4)
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo
  9. customThe crude residue was purified by chromatography on silica gel with dichloromethane

Quellen und Nachweise

ORD-Eintrag
ord-8e91cf9cd14643fd875cfb996a410ca8
Quelldatensatz
uspto-grants-2010_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07807686B2

Notizen zur Reaktion

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