Dimethyl Sulfoxide → HCID 70620955、化合物

HRID 2420470ノート

反応式

HRID 2420470 の反応式
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][CH:9]([NH:11][CH2:12][CH2:13][CH:14]([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)[C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[CH3:10])=[CH:4][CH:3]=1.[OH-:27].[Na+].CS(C)=[O:31].[CH3:33][C:34]1[CH:35]=[CH:36][C:37]([CH2:40]Cl)=[N:38][CH:39]=1.[OH2:42]>>[C:2]([OH:1])(=[O:31])/[CH:7]=[CH:6]\[C:5]([OH:42])=[O:27].[CH3:33][C:34]1[CH:35]=[CH:36][C:37]([CH2:40][O:1][C:2]2[CH:3]=[CH:4][C:5]([CH2:8][CH:9]([NH:11][CH2:12][CH2:13][CH:14]([C:21]3[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=3)[C:15]3[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=3)[CH3:10])=[CH:6][CH:7]=2)=[N:38][CH:39]=1

参加物

6

反応物 5

HCID 679Dimethyl SulfoxideHCID 962WaterHCID 14798Sodium HydroxideHCID 5880562-(Chloromethyl)-5-methylpyridineHCID 130652814-{2-[(3,3-Diphenylpropyl)amino]propyl}phenol

生成物 1

HCID 70620955HCID 70620955、化合物

実験手順

The mixture of 21.76 g of dl-1-(4-hydroxyphenyl)-2-(3,3-diphenylpropylamino)-propane, 6.3 ml of 10 N aqueous sodium hydroxide and 100 ml of dimethylsulphoxide is stirred at 60° for 2 hours, whereupon 8.91 g of 5-methyl-2-pyridylmethyl chloride are added. The whole is stirred at ambient temperature for 24 hours, diluted with 400 ml of water and extracted with methylene chloride. The extract is dried, evaporated, the residual oil taken up in isopropanol and the solution acidified with maleic acid in isopropanol until the pH of 5 is reached, to yield the dl-1-[4-(5-methyl-2-pyridylmethoxy)-phenyl]-2-(3,3-diphenylpropylamino)propane maleate, melting at 155°-157°.

後処理

  1. additionare added
  2. extractionextracted with methylene chloride
  3. customThe extract is dried
  4. customevaporated

出典と根拠

ORDレコード
ord-d344c61602c945d581a4f0b1d3be333a
出典データセット
uspto-grants-1978_08
特許番号
US04110457

反応ノート

読み込み中…