Triphenylphosphine → HCID 86641939, 화합물

HRID 384109노트

반응식

HRID 384109 반응식
[Br:1][C:2]1[N:7]=[CH:6][C:5]([OH:8])=[CH:4][CH:3]=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.N(C(OCC)=O)=NC(OCC)=O.[O:40]([C:47]1[CH:52]=[CH:51][CH:50]=[CH:49][C:48]=1[CH2:53]O)[C:41]1[CH:46]=[CH:45][CH:44]=[CH:43][CH:42]=1>O1CCCC1>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([O:8][CH2:53][C:48]2[CH:49]=[CH:50][CH:51]=[CH:52][C:47]=2[O:40][C:41]2[CH:46]=[CH:45][CH:44]=[CH:43][CH:42]=2)=[CH:6][N:7]=1

참가 물질

6

반응물 4

HCID 11776TriphenylphosphineHCID 220568ethyl N-ethoxycarbonyliminocarbamateHCID 27628652-Bromo-5-hydroxypyridineHCID 36601112-Phenoxybenzyl alcohol

생성물 1

HCID 86641939HCID 86641939, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 6-bromopyridin-3-ol (1.76 g) in tetrahydrofuran (20 ml), 3.20 g of triphenylphosphine, 5.52 ml of diethyl azodicarboxylate (45% toluene solution) and 2.43 g of (2-phenoxyphenyl)methanol were added, and the reaction solution was stirred overnight at room temperature. The reaction solvent was distilled off under reduced pressure, and the residue obtained was purified by silica gel column chromatography (eluent: ethyl acetate/hexane (0:100-15:85)) to afford the title compound as a yellow oil.

후처리

  1. distillationThe reaction solvent was distilled off under reduced pressure
  2. customthe residue obtained
  3. customwas purified by silica gel column chromatography (eluent: ethyl acetate/hexane (0:100-15:85))

출처 및 근거

ORD 기록
ord-a6bb457da661413a8ea1867335fcd100
출처 데이터셋
uspto-grants-2013_02
특허 번호
US08367708B2

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