Triphenylphosphine → HCID 86641939、化合物

HRID 384109ノート

反応式

HRID 384109 の反応式
[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

参加物

6

反応物 4

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

生成物 1

HCID 86641939HCID 86641939、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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))

出典と根拠

ORDレコード
ord-a6bb457da661413a8ea1867335fcd100
出典データセット
uspto-grants-2013_02
特許番号
US08367708B2

反応ノート

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