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Triethylamine → 1-benzyl-N-hydroxy-4-(4-methoxyphenylsulfonyl)piperidine-4-carboxamide

HRID 1531078
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Reaktionsgleichung

Reaktionsgleichung von HRID 1531078
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([S:9]([C:12]2([C:25]([OH:27])=O)[CH2:17][CH2:16][N:15]([CH2:18][C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)[CH2:14][CH2:13]2)(=[O:11])=[O:10])=[CH:5][CH:4]=1.C(Cl)(=O)C(Cl)=O.Cl.[NH2:35][OH:36].C(N(CC)CC)C>CN(C=O)C.C(Cl)Cl.C1COCC1.O>[OH:36][NH:35][C:25]([C:12]1([S:9]([C:6]2[CH:7]=[CH:8][C:3]([O:2][CH3:1])=[CH:4][CH:5]=2)(=[O:11])=[O:10])[CH2:17][CH2:16][N:15]([CH2:18][C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[CH2:14][CH2:13]1)=[O:27]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 4

HCID 8471TriethylamineHCID 65578Oxalyl chloride2×HCID 443297Hydroxyamine hydrochlorideHCID 111436104-(4-Methoxy-benzenesulfonyl)-1-benzyl-piperidine-4-carboxylic acid

Produkt 1

HCID 98659361-benzyl-N-hydroxy-4-(4-methoxyphenylsulfonyl)piperidine-4-carboxamide

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 6228DimethylformamideKatalysator
HCID 6344DichloromethaneLösungsmittel
HCID 21881883Oxolane--water (1/1)Lösungsmittel

Versuchsvorschrift

To a stirred solution of 4-(4-Methoxy-benzenesulfonyl)-1-benzyl-piperidine-4-carboxylic acid (2.0 g, 5.1 mmol) and DMF (2 drops) in CH2Cl2 (100 ml) at 0° C., oxalyl chloride (1.0 gm, 8 mmol) was added in a drop-wise manner. After the addition, the reaction mixture was stirred at room temperature for 1 hour. Simultaneously, in a separate flask a mixture of hydroxylamine hydrochloride (2.0 gm, 29 mmol) and triethylamine (5 ml, excess) was stirred in THF:water (5:1, 30 ml) at 0° C. for 1 hour. At the end of 1 hour, the oxalyl chloride reaction mixture was concentrated and the pale yellow residue was dissolved in 10 ml of CH2Cl2 and added slowly to the hydroxylamine at 0° C. The reaction mixture was stirred at room temperature for 24 hours and concentrated. The residue obtained was extracted with chloroform and washed well with water. The product obtained was purified by silica gel column chromatography and eluted with chloroform the product 4-(4-Methoxy-benzenesulfonyl)-1-benzyl-piperidine-4-carboxylic acid hydroxyamide was isolated as a colorless solid. mp 90-95° C.; Yield, 1.2 g, 48%; MS: 405 (M+H)+; 1H NMR (300 MHz, DMSO-d6): δ 2.29 (m, 3H), 2.76-2.79 (m, 2H), 3.43 (m, 4H),4.30 (s, 2H), 7.14-7.17 (d,2H), 7.50-7.73 (m, 5H), 9.37 (s, 1H), 10.53 (s, 1H), 11.18 (s, 1H).

Aufarbeitung

  1. additionAfter the addition
  2. concentrationwas concentrated
  3. dissolutionthe pale yellow residue was dissolved in 10 ml of CH2Cl2
  4. additionadded slowly to the hydroxylamine at 0° C
  5. stirringThe reaction mixture was stirred at room temperature for 24 hours
  6. concentrationconcentrated
  7. customThe residue obtained
  8. extractionwas extracted with chloroform
  9. washwashed well with water
  10. customThe product obtained
  11. customwas purified by silica gel column chromatography
  12. washeluted with chloroform the product 4-(4-Methoxy-benzenesulfonyl)-1-benzyl-piperidine-4-carboxylic acid hydroxyamide
  13. customwas isolated as a colorless solid
  14. customYield

Quellen und Nachweise

ORD-Eintrag
ord-0dfef0a19bd24d368e21d8ea94409275
Quelldatensatz
uspto-grants-2001_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06197791B1

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