Pyridine → N-(11-Carbomethoxyundecanoyl)-2-hydroxyaniline

HRID 1290717노트

반응식

HRID 1290717 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[OH:8].N1C=CC=CC=1.[C:15]([O:30][CH3:31])(=[O:29])[CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][C:26]([O-])=[O:27]>C(Cl)Cl>[C:15]([CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][C:26]([NH:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[OH:8])=[O:27])([O:30][CH3:31])=[O:29]

참가 물질

5

반응물 3

HCID 1049PyridineHCID 58012-AminophenolHCID 22672980Dodecanedioic acid, monomethyl ester

생성물 1

HCID 18795789N-(11-Carbomethoxyundecanoyl)-2-hydroxyaniline

시약·촉매·용매 1

HCID 6344Dichloromethane용매3회

실험 절차

To a stirred near solution of 2-aminophenol (0.24 g, 2.2 mM) in anhydrous methylene chloride (25 mL) was added dry pyridine (0.66 mL) and the mixture cooled in an ice-water bath. A solution of (7) (0.525 g, 2.0 mM) in methylene chloride (2 mL) was added over 1 minute (2×1.5 mL methylene chloride rinses), and the mixture allowed to stir cold. After 30 minutes the bath was removed. After stirring overnight at ambient temperatures, the mixture was filtered, the solvents removed in vacuo, and the residue pumped to remove all traces of pyridine. The product, (44) was used as is in subsequent steps.

후처리

  1. temperaturethe mixture cooled in an ice-water bath
  2. customAfter 30 minutes the bath was removed
  3. stirringAfter stirring overnight at ambient temperatures
  4. filtrationthe mixture was filtered
  5. customthe solvents removed in vacuo
  6. customto remove all traces of pyridine

출처 및 근거

ORD 기록
ord-d0b992ae376147b9b6b103338a8fd4ff
출처 데이터셋
uspto-grants-1998_05
특허 번호
US05753641

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