对甲苯磺酸 → 三苯基氧化膦

HRID 4116

反应方程式

HRID 4116 反应方程式
C1(C)C=CC(S(O)(=O)=[O:8])=CC=1.[O:12]=[C:13]1[C:18]([O:19][CH2:20][C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)=[CH:17][NH:16][C:15]([CH:27](O)OC)=[CH:14]1.[CH2:31]([O:33][C:34](=[O:55])[CH:35]=[P:36]([C:49]1[CH:54]=[CH:53][CH:52]=[CH:51][CH:50]=1)([C:43]1[CH:48]=[CH:47][CH:46]=[CH:45][CH:44]=1)[C:37]1[CH:42]=[CH:41][CH:40]=[CH:39][CH:38]=1)[CH3:32]>>[O:12]=[C:13]1[C:18]([O:19][CH2:20][C:21]2[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=2)=[CH:17][NH:16][C:15](/[CH:27]=[CH:35]/[C:34]([O:33][CH2:31][CH3:32])=[O:55])=[CH:14]1.[C:49]1([P:36](=[O:8])([C:43]2[CH:44]=[CH:45][CH:46]=[CH:47][CH:48]=2)[C:37]2[CH:38]=[CH:39][CH:40]=[CH:41][CH:42]=2)[CH:54]=[CH:53][CH:52]=[CH:51][CH:50]=1

参与物

5

反应物 3

HCID 6101对甲苯磺酸HCID 70670乙氧甲酰基亚甲基三苯基膦HCID 141825172-(1-hydroxy-1-methoxymethyl)-5-(phenylmethoxy)-4(1H)-pyridinone

产物 2

HCID 13097三苯基氧化膦HCID 14182518(E)-3-[1,4-Dihydro-4-oxo-5-(phenylmethoxy)-2-pyridinyl]-2-propenoic acid, ethyl ester

实验过程

p-Toluenesulfonic acid (0.5 g), 6.26 g of 1,4-dihydro-4-oxo-2-[(hydroxy)(methoxy)methyl]-5-(phenylmethoxy)pyridine and 8.35 g of (triphenylphosphoranylidene)acetic acid ethyl ester were stirred for three hours at 70° C. A clear dark solution was formed. Evaporation of the solvent in vacuo yielded an oily residue of the title compound and triphenylphosphine oxide. This was dissolved in 30 ml of isopropanol. After standing overnight in a refrigerator, the resulting crystals were filtered off, washed with ether and recrystallized from isopropanol (yield: 5.72 g).

后处理

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

来源与证据

ORD记录
ord-412af217645140608f36a96b6d5ec195
来源数据集
uspto-grants-1988_02
专利号
US04723002

关联笔记

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