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1-Octanol → HCID 178443705, 화합물

HRID 1780569
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HRID 1780569 반응식
N(C(OCC)=O)=NC(OCC)=O.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[F:32][C:33]1[C:38]([OH:39])=[CH:37][CH:36]=[C:35]([C:40]2[CH:45]=[CH:44][C:43]([C@H:46]3[CH2:51][CH2:50][C@H:49]([CH2:52][CH2:53][CH2:54][CH2:55][CH3:56])[CH2:48][CH2:47]3)=[CH:42][CH:41]=2)[N:34]=1.[CH2:57](O)[CH2:58][CH2:59][CH2:60][CH2:61][CH2:62][CH2:63][CH3:64]>O1CCCC1>[F:32][C:33]1[C:38]([O:39][CH2:57][CH2:58][CH2:59][CH2:60][CH2:61][CH2:62][CH2:63][CH3:64])=[CH:37][CH:36]=[C:35]([C:40]2[CH:45]=[CH:44][C:43]([C@H:46]3[CH2:51][CH2:50][C@H:49]([CH2:52][CH2:53][CH2:54][CH2:55][CH3:56])[CH2:48][CH2:47]3)=[CH:42][CH:41]=2)[N:34]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 9571-OctanolHCID 11776TriphenylphosphineHCID 220568ethyl N-ethoxycarbonyliminocarbamateHCID 178444290HCID 178444290, 화합물

생성물 1

HCID 178443705HCID 178443705, 화합물수율 48.4%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran
용매

실험 절차

0.26 g (1.50 mmol) of diethyl azodicarboxylate is added dropwise at 0° C. to 0.39 g (1.50 mmol) of triphenylphosphine in 10 ml of tetrahydrofuran, and the mixture is stirred at room temperature for 30 minutes. 0.31 g (0.91 mmol) of 2-fluoro-3-hydroxy-6-[4-(trans-4-pentylcyclohexyl)phenyl]pyridine and 0.19 g (1.50 mmol) of 1-octanol are then added. After a reaction time of 2hours at room temperature, the solvent is distilled off, and the residue is purified by chromatography (silica gel, 9:1 hexane/ethyl acetate) and by recrystallization from acetonitrile, giving 0.20 g of 2-fluoro-3-octyloxy-6-[4-(trans-4-pentylcyclohexyl)phenyl]pyridine. ##STR52##

후처리

  1. distillationAfter a reaction time of 2hours at room temperature, the solvent is distilled off
  2. customthe residue is purified by chromatography (silica gel, 9:1 hexane/ethyl acetate) and by recrystallization from acetonitrile

출처 및 근거

ORD 기록
ord-f884640e437c4aaba7d430b3beb6dbeb
출처 데이터셋
uspto-grants-1997_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05630962

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