p-Toluenesulfonic acid → Triphenylphosphine Oxide

HRID 1252628

反応式

HRID 1252628 の反応式
C1(C)C=CC(S(O)(=O)=[O:8])=CC=1.O[CH:13]([C:16]1[NH:17][CH:18]=[C:19]([O:23][CH2:24][C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)[C:20](=[O:22])[CH:21]=1)OC.[C:31]([CH:36]=[P:37]([C:50]1[CH:55]=[CH:54][CH:53]=[CH:52][CH:51]=1)([C:44]1[CH:49]=[CH:48][CH:47]=[CH:46][CH:45]=1)[C:38]1[CH:43]=[CH:42][CH:41]=[CH:40][CH:39]=1)([O:33][CH2:34][CH3:35])=[O:32]>O1CCOCC1>[O:22]=[C:20]1[C:19]([O:23][CH2:24][C:25]2[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=2)=[CH:18][NH:17][C:16]([CH:13]=[CH:36][C:31]([O:33][CH2:34][CH3:35])=[O:32])=[CH:21]1.[C:50]1([P:37](=[O:8])([C:44]2[CH:49]=[CH:48][CH:47]=[CH:46][CH:45]=2)[C:38]2[CH:39]=[CH:40][CH:41]=[CH:42][CH:43]=2)[CH:55]=[CH:54][CH:53]=[CH:52][CH:51]=1

参加物

6

反応物 3

HCID 6101p-Toluenesulfonic acidHCID 70670Acetic acid, 2-(triphenylphosphoranylidene)-, ethyl esterHCID 141825172-(1-hydroxy-1-methoxymethyl)-5-(phenylmethoxy)-4(1H)-pyridinone

生成物 2

HCID 13097Triphenylphosphine OxideHCID 86742168HCID 86742168、化合物

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

0.5 g of p-toluenesulfonic acid, 6.26 g of 2-(1-hydroxy-1-methoxymethyl)-5-(phenylmethoxy)-4(1H)-pyridinone and 8.35 g of carbethoxymethylenetriphenylphosphorane were stirred for 3 hours in 100 ml of dioxane at 70° C. A clear, dark-colored solution was formed. Evaporation of the solvent in vacuo yielded an oily residue of the title compound and triphenylphosphine oxide. The residue was dissolved in 30 ml of isopropanol and crystals of product began to separate. After standing in a refrigerator overnight, the crystals were filtered off, washed with ether and recrystallized from isopropanol. Yield: 5.72 g, melting point 188° C.

後処理

  1. customA clear, dark-colored solution was formed
  2. customEvaporation of the solvent in vacuo

出典と根拠

ORDレコード
ord-a908bb603e0146ed9a83ce1678d4b7aa
出典データセット
uspto-grants-1988_05
特許番号
US04743685

関連ノート

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