Sodium hydride → N,N-Dimethyl-3-{2-[4-(2-methoxyphenyl)butyl]phenoxy}propylamine

HRID 743208노트

반응식

HRID 743208 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[CH2:9][CH2:10][CH2:11][CH2:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=1[OH:19].[H-].[Na+].Cl.[CH3:23][N:24]([CH3:29])[CH2:25][CH2:26][CH2:27]Cl>CC(N(C)C)=O>[CH3:23][N:24]([CH2:25][CH2:26][CH2:27][O:19][C:14]1[CH:15]=[CH:16][CH:17]=[CH:18][C:13]=1[CH2:12][CH2:11][CH2:10][CH2:9][C:4]1[CH:5]=[CH:6][CH:7]=[CH:8][C:3]=1[O:2][CH3:1])[CH3:29]

참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 943083-(Dimethylamino)propyl chloride hydrochlorideHCID 194239792-[4-(2-Methoxyphenyl)butyl]phenol

생성물 1

HCID 19423881N,N-Dimethyl-3-{2-[4-(2-methoxyphenyl)butyl]phenoxy}propylamine수율 85.2%

시약·촉매·용매 1

HCID 31374Dimethylacetamide용매

실험 절차

Following a procedure similar to that described in Example 2(a), 200 mg of 2-[4-(2-methoxyphenyl)butyl]phenol (prepared as described in Preparation 4), 75 mg of sodium hydride (as a 55% w/w dispersion in mineral oil) and 0.14 g of 3-dimethylaminopropyl chloride hydrochloride were reacted in 20 ml of dimethylacetamide. The crude product, extracted as described in Example 2(a), was purified by column chromatography through silica gel, using a 10:1 by volume mixture of methylene chloride and methanol as the eluent, to give 227 mg (yield 85%) of the title compound as pale yellow solid.

후처리

  1. extractionThe crude product, extracted
  2. customwas purified by column chromatography through silica gel
  3. additionby volume mixture of methylene chloride and methanol as the eluent

출처 및 근거

ORD 기록
ord-79e7a6ecc7db4a0083533a7b5786e19a
출처 데이터셋
uspto-grants-1996_09
특허 번호
US05556864

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