Triethylamine → N,O-dimethyl-N-(1-trityl-piperidine-4-carbonyl)hydroxylamine

HRID 278571

반응식

HRID 278571 반응식
[C:1]([N:20]1[CH2:25][CH2:24][CH:23]([C:26]([OH:28])=O)[CH2:22][CH2:21]1)([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl.[CH3:30][O:31][NH:32][CH3:33].C(N(CC)CC)C.CCN=C=NCCCN(C)C>ClCCl>[CH3:33][N:32]([O:31][CH3:30])[C:26]([CH:23]1[CH2:22][CH2:21][N:20]([C:1]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)([C:2]2[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=2)[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=2)[CH2:25][CH2:24]1)=[O:28]

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 81138Methanamine, N-methoxy-, hydrochloride (1:1)HCID 205201821-Tritylpiperidine-4-carboxylic acid

생성물 1

HCID 22628088N,O-dimethyl-N-(1-trityl-piperidine-4-carbonyl)hydroxylamine

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a mixture of 1-tritylpiperidine-4-carboxylic acid (7.0 g), O,N-dimethylhydroxylamine hydrochloride (2.0 g) and triethylamine (2.9 ml) in dichloromethane (70 ml) was added WSC (3.97 g), and the mixture was stirred at room temperature for 1 hour and concentrated. To the residue was added ethyl acetate, and the mixture was washed with water, dried (MgSO4) and concentrated. The resulting crystals (6.3 g) were washed with isopropylether.

후처리

  1. concentrationconcentrated
  2. additionTo the residue was added ethyl acetate
  3. washthe mixture was washed with water
  4. dry with materialdried (MgSO4)
  5. concentrationconcentrated
  6. washThe resulting crystals (6.3 g) were washed with isopropylether

출처 및 근거

ORD 기록
ord-13e3f414752049a18edaff60a4782d74
출처 데이터셋
uspto-grants-2002_03
특허 번호
US06359134B1

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