2-(Dimethylamino)ethanol → 2-[3-(2-Dimethylaminoethoxy)propyl]-5-methoxymethoxy-4,6,7-trimethyl-1,3-benzoxathiole

HRID 2308882ノート

反応式

HRID 2308882 の反応式
[CH3:1][N:2]([CH3:6])[CH2:3][CH2:4][OH:5].[H-].[Na+].Br[CH2:10][CH2:11][CH2:12][CH:13]1[S:17][C:16]2[C:18]([CH3:28])=[C:19]([O:24][CH2:25][O:26][CH3:27])[C:20]([CH3:23])=[C:21]([CH3:22])[C:15]=2[O:14]1>CS(C)=O>[CH3:1][N:2]([CH3:6])[CH2:3][CH2:4][O:5][CH2:10][CH2:11][CH2:12][CH:13]1[S:17][C:16]2[C:18]([CH3:28])=[C:19]([O:24][CH2:25][O:26][CH3:27])[C:20]([CH3:23])=[C:21]([CH3:22])[C:15]=2[O:14]1

参加物

5

反応物 3

HCID 79022-(Dimethylamino)ethanolHCID 24758Sodium hydrideHCID 148021932-(3-Bromopropyl)-5-methoxymethoxy-4,6,7-trimethyl-1,3-benzoxathiole

生成物 1

HCID 148021942-[3-(2-Dimethylaminoethoxy)propyl]-5-methoxymethoxy-4,6,7-trimethyl-1,3-benzoxathiole

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒2 回

反応条件

温度
50 °C

実験手順

740 mg of 2-dimethylaminoethanol were dissolved in 10 ml of dimethyl sulfoxide, and 220 mg of a 50% w/w oily suspension of sodium hydride was added to the resulting solution; the reaction mixture was then heated at 50° C. for 1 hour, after which it was cooled down with ice, and a solution of 1.68 g of 2-(3-bromopropyl)-5-methoxymethoxy-4,6,7-trimethyl-1,3-benzoxathiole (prepared as described in Example 87) in 5 ml of dimethyl sulfoxide was added dropwise, while stirring. The reaction product was then subjected to the same reaction process, extraction and separation procedures as described in (a) above, to give the title compound with the same Rf value and mass spectrum as those of the product obtained in (a).

後処理

  1. additionwas added to the resulting solution
  2. temperatureafter which it was cooled down with ice
  3. extractionThe reaction product was then subjected to the same reaction process, extraction and separation procedures

出典と根拠

ORDレコード
ord-cfe94c73ab5d48ed966e040e4e4e1855
出典データセット
uspto-grants-1987_09
特許番号
US04691027

反応ノート

読み込み中…