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

HRID 991081
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HRID 991081 반응식
[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>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]
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참가 물질

7

반응물 4

HCID 8471TriethylamineHCID 65578Oxalyl chloride2회HCID 443297Hydroxyamine hydrochlorideHCID 111436104-(4-Methoxy-benzenesulfonyl)-1-benzyl-piperidine-4-carboxylic acid

생성물 1

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

시약·촉매·용매 2

HCID 6344
Dichloromethane
용매
HCID 21881883Oxolane--water (1/1)용매

실험 절차

To a stirred solution of 4-(4-Methoxy-benzenesulfonyl)-1-benzyl-piperidine-4-carboxylic acid (2.0 g, 5.1 mmol) and DMEF (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 miture 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).

후처리

  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

출처 및 근거

ORD 기록
ord-5ce15bd570c84d039fd59092fcd15e36
출처 데이터셋
uspto-grants-2002_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06462073B2

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