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3-Hydroxypyridine → 4-(3-Pyridyloxymethyl)2-phenylbenzoic acid methyl ester

HRID 2121195
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인쇄 미리보기

반응식

HRID 2121195 반응식
[OH:1][C:2]1[CH:3]=[N:4][CH:5]=[CH:6][CH:7]=1.C[Si](C)(C)[N-][Si](C)(C)C.[K+].C1OCCOCCOCCOCCOCCOC1.[CH3:36][O:37][C:38](=[O:53])[C:39]1[CH:44]=[CH:43][C:42]([CH2:45]Br)=[CH:41][C:40]=1[C:47]1[CH:52]=[CH:51][CH:50]=[CH:49][CH:48]=1>COCCOC.C1(C)C=CC=CC=1.O>[CH3:36][O:37][C:38](=[O:53])[C:39]1[CH:44]=[CH:43][C:42]([CH2:45][O:1][C:2]2[CH:3]=[N:4][CH:5]=[CH:6][CH:7]=2)=[CH:41][C:40]=1[C:47]1[CH:48]=[CH:49][CH:50]=[CH:51][CH:52]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 79713-HydroxypyridineHCID 2855718-Crown-6HCID 3251421Potassium bis(trimethylsilyl)amideHCID 18474540Methyl 4-bromomethyl-2-phenylbenzoate

생성물 1

HCID 106870984-(3-Pyridyloxymethyl)2-phenylbenzoic acid methyl ester수율 48.4%

시약·촉매·용매 3

HCID 962
Water
용매
HCID 1140Toluene용매
HCID 80711,2-Dimethoxyethane용매

실험 절차

To a mechanically-stirred 0° C. solution of 3-hydroxypyridine (4.4 g, 46 mmol) in DME (20 mL) was added potassium hexamethyldisilazide (0.5 M in toluene, 88.5 mL, 44 mmol) and the mixture was stirred for 15 minutes. 18-Crown-6 (1.46 g, 5.5 mmol) and a solution of 4-bromomethyl-2-phenylbenzoic acid methyl ester (6.8 g, 22 mmol) in toluene (25 mL) was added and the reaction mixture was vigorously stirred overnight. The reaction mixture was poured into 200 mL of water and the layers were separated. The aqueous phase was extracted with 2 portions of ethyl acetate and the combined organic phases were extracted with water and brine, dried (MgSO4), filtered and concentrated. The resulting oil was purified by flash chromatography (65% ethyl acetate-hexane) to give 4-(3-pyridyloxymethyl)-2-phenylbenzoic acid methyl ester (3.4 g).

후처리

  1. waitthe reaction mixture was vigorously stirred overnight
  2. customthe layers were separated
  3. extractionThe aqueous phase was extracted with 2 portions of ethyl acetate
  4. extractionthe combined organic phases were extracted with water and brine
  5. dry with materialdried (MgSO4)
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customThe resulting oil was purified by flash chromatography (65% ethyl acetate-hexane)

출처 및 근거

ORD 기록
ord-46f1714deabd407f83f5d6ccbca48c2c
출처 데이터셋
uspto-grants-2004_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06693123B2

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