Sodium Iodide → 4(1H)-Pyridinone, 1,5-bis(diphenylmethoxy)-2-(hydroxymethyl)-

HRID 620750ノート

反応式

HRID 620750 の反応式
[OH:1][N:2]1[CH:7]=[C:6]([O:8][CH:9]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[C:5](=[O:22])[CH:4]=[C:3]1[CH2:23][OH:24].C(=O)([O-])[O-].[K+].[K+].[I-].[Na+].[CH:33](Cl)([C:40]1[CH:45]=[CH:44][CH:43]=[CH:42][CH:41]=1)[C:34]1[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=1>CS(C)=O>[CH:33]([O:1][N:2]1[CH:7]=[C:6]([O:8][CH:9]([C:16]2[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=2)[C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[C:5](=[O:22])[CH:4]=[C:3]1[CH2:23][OH:24])([C:34]1[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=1)[C:40]1[CH:45]=[CH:44][CH:43]=[CH:42][CH:41]=1

参加物

6

反応物 4

HCID 5238Sodium IodideHCID 7035ChlorodiphenylmethaneHCID 11430Potassium CarbonateHCID 143063884(1H)-Pyridinone, 5-(diphenylMethoxy)-1-hydroxy-2-(hydroxyMethyl)-

生成物 1

HCID 117521734(1H)-Pyridinone, 1,5-bis(diphenylmethoxy)-2-(hydroxymethyl)-収率 100%

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

反応条件

温度
100 °C

実験手順

8.1 g (0.0251 mol) of the product of Step (2) was added to dimethylsulfoxide (125 ml) and heated to 100° C. and dissolved. After cooling the solution to room temperature, 5.2 g (0.0375 mol) of potassium carbonate and 5.6 g (0.0375 mol) of sodium iodide and 6.7 ml (0.0375 mol) of benzhydrylchloride were added thereto, and the mixture was reacted at room temperature for 18 hours under stirring. To the reaction solution, ice water was gradually added, and formed precipitates were collected by filtration, washed sequentially with water and ethyl ether/n-hexane (2/1), and dried to obtain 12.3 g (yield: 100%) of the above identified compound.

後処理

  1. dissolutiondissolved
  2. temperatureAfter cooling the solution to room temperature
  3. customthe mixture was reacted at room temperature for 18 hours
  4. customformed
  5. customprecipitates
  6. filtrationwere collected by filtration
  7. washwashed sequentially with water and ethyl ether/n-hexane (2/1)
  8. customdried
  9. customto obtain 12.3 g (yield: 100%) of the

出典と根拠

ORDレコード
ord-6e75ba8a6cd64955a2afbfdd15dcfa17
出典データセット
uspto-grants-1989_04
特許番号
US04822786

反応ノート

読み込み中…