Water → HCID 19006234, 화합물

HRID 1743032노트

반응식

HRID 1743032 반응식
[H-].[Na+].[N:3]1[CH:8]=[CH:7][CH:6]=[C:5]([C:9]2[C:18]3[C:13](=[CH:14][C:15]([O:21][CH3:22])=[C:16]([O:19][CH3:20])[CH:17]=3)[CH:12]=[C:11]([CH2:23][OH:24])[C:10]=2[CH2:25][OH:26])[CH:4]=1.S(C1C=CC(C)=CC=1)(O[CH2:31][C:32]([CH3:35])([CH3:34])[CH3:33])(=O)=O.O>CN(C)P(=O)(N(C)C)N(C)C>[N:3]1[CH:8]=[CH:7][CH:6]=[C:5]([C:9]2[C:18]3[C:13](=[CH:14][C:15]([O:21][CH3:22])=[C:16]([O:19][CH3:20])[CH:17]=3)[CH:12]=[C:11]([CH2:23][O:24][CH2:31][C:32]([CH3:35])([CH3:34])[CH3:33])[C:10]=2[CH2:25][OH:26])[CH:4]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 24758Sodium hydrideHCID 283345Neopentyl tosylateHCID 15224777HCID 15224777, 화합물

생성물 1

HCID 19006234HCID 19006234, 화합물

시약·촉매·용매 1

HCID 12679Hexamethylphosphoramide용매2회

실험 절차

To a suspension of sodium hydride in hexamethylphosphoric triamide (40 ml) is added a solution of 1-(3-pyridyl)-2,3-bis(hydroxymethyl)-6,7-dimethoxynaphthalene in hexamethylphosphoramide (10 ml) under ice-cooling. The mixture is warmed to room temperature, and then stirred for 30 minutes. To the reaction solution is added neo-pentyl tosylate (3.67 g), and the mixture is reacted at 100° C. for 30 minutes. The mixture is allowed to cool, and thereto is added water, and the mixture is extracted with ethyl acetate. The extract is washed with water, dried, and concentrated. The resulting residue is subjected to silica gel column chromatography (eluent; chloroform:acetone=5:1), and the desired fractions are concentrated to give 1-(3-pyridyl)-2-hydroxymethyl-3-neo-pentyloxymethyl-6,7-dimethoxynaphthalene (1.5 g) as an oily product.

후처리

  1. temperaturecooling
  2. customthe mixture is reacted at 100° C. for 30 minutes
  3. temperatureto cool
  4. extractionthe mixture is extracted with ethyl acetate
  5. washThe extract is washed with water
  6. customdried
  7. concentrationconcentrated
  8. concentrationthe desired fractions are concentrated

출처 및 근거

ORD 기록
ord-4acd29f9f95a4b0b90e121a352cda0ce
출처 데이터셋
uspto-grants-1994_08
특허 번호
US05342941

반응 노트

불러오는 중…