Sodium hydride → 4-{2-[2-(4-Phenylbutyl)phenoxy]ethyl}morpholine

HRID 743180노트

반응식

HRID 743180 반응식
[C:1]1([CH2:7][CH2:8][CH2:9][CH2:10][C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2[OH:17])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Cl.Cl[CH2:20][CH2:21][N:22]1[CH2:27][CH2:26][O:25][CH2:24][CH2:23]1.[H-].[Na+]>CC(N(C)C)=O>[C:1]1([CH2:7][CH2:8][CH2:9][CH2:10][C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2[O:17][CH2:20][CH2:21][N:22]2[CH2:27][CH2:26][O:25][CH2:24][CH2:23]2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 77210Morpholine, 4-(2-chloroethyl)-, hydrochloride (1:1)HCID 125964892-(4-Phenylbutyl)phenol

생성물 1

HCID 153890304-{2-[2-(4-Phenylbutyl)phenoxy]ethyl}morpholine수율 76.5%

시약·촉매·용매 1

HCID 31374Dimethylacetamide용매

실험 절차

Following a procedure similar to that described in Example 2, 340 mg of 2-(4-phenylbutyl)phenol (prepared as described in Preparation 3), 330 mg of 4-(2-chloroethyl)morpholine hydrochloride and 140 mg of sodium hydride (as a 55% w/w dispersion in mineral oil) were reacted in 20 ml of dimethylacetamide. The crude product, extracted as described in Example 2, was purified by column chromatography through silica gel, using a 3:2 by volume mixture of ethyl acetate and hexane as the eluent, to give 390 mg (yield 76%) of the title compound as a colorless oil.

후처리

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

출처 및 근거

ORD 기록
ord-fd6061f4037640b5b3e6cd934643dc81
출처 데이터셋
uspto-grants-1996_09
특허 번호
US05556864

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