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Triethylamine → HCID 19046971, 화합물

HRID 1780572
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HRID 1780572 반응식
[F:1][C:2]1[C:7]([CH:8]=[O:9])=[CH:6][CH:5]=[C:4]([C:10]2[CH:15]=[CH:14][C:13]([O:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH3:24])=[CH:12][CH:11]=2)[N:3]=1.[CH2:25]([CH:33]([CH2:36]O)[CH2:34][OH:35])[CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH3:32].S([O-])([O-])(=O)=O.[Na+].[Na+].C(N(CC)CC)C>C1(C)C=CC=CC=1.C1(C)C=CC(S(O)(=O)=O)=CC=1>[F:1][C:2]1[C:7]([CH:8]2[O:35][CH2:34][CH:33]([CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH3:32])[CH2:36][O:9]2)=[CH:6][CH:5]=[C:4]([C:10]2[CH:15]=[CH:14][C:13]([O:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH3:24])=[CH:12][CH:11]=2)[N:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 8471TriethylamineHCID 24436Sodium SulfateHCID 3160622-Octylpropane-1,3-diolHCID 19046983HCID 19046983, 화합물

생성물 1

HCID 19046971HCID 19046971, 화합물수율 41.9%

시약·촉매·용매 2

HCID 6101p-Toluenesulfonic acid촉매
HCID 1140Toluene용매

실험 절차

2.20 g (6.68 mmol) of 2-fluoro-3-formyl-6-(4-octyloxyphenyl)pyridine, 1.26 g (6.68 mmol) of 2-octylpropane-1,3-diol, 0.02g (0.10mmol) of p-toluenesulfonic acid and 3.00 g of sodium sulfate are stirred in 100 ml of toluene at room temperature for 68 hours. 0.14 ml (1.00 mmol) of triethylamine is then added, sodium sulfate is filtered off, the filtrate is concentrated, and the residue is purified by chromatography (silica gel, 9:1 hexane/ethyl acetate) and by recrystallization from acetonitrile, giving 1.40 g of 2-fluoro-3-(5-octyl-1,3-dioxane-2-yl)-6-(4-octyloxyphenyl)pyridine. ##STR63##

후처리

  1. filtrationsodium sulfate is filtered off
  2. concentrationthe filtrate is concentrated
  3. customthe residue is purified by chromatography (silica gel, 9:1 hexane/ethyl acetate) and by recrystallization from acetonitrile

출처 및 근거

ORD 기록
ord-9e14d2b82bf140c8b1d4d29f7c8e42bd
출처 데이터셋
uspto-grants-1997_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05630962

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