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

HRID 278571

反応式

HRID 278571 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-13e3f414752049a18edaff60a4782d74
出典データセット
uspto-grants-2002_03
特許番号
US06359134B1

関連ノート

読み込み中…