N,N-Dimethylcyclohexylamine → 2,5-Dimethyl-3-[(pyridin-3-yl)oxy]-1lambda~6~,2,4,6-thiatriazine-1,1(2H)-dione

HRID 1381059ノート

反応式

HRID 1381059 の反応式
[CH:1]1[CH:6]=[N:5][CH:4]=[C:3]([OH:7])[CH:2]=1.CN(C1CCCCC1)C.[CH3:17][N:18]1[C:23](Cl)=[N:22][C:21]([CH3:25])=[N:20][S:19]1(=[O:27])=[O:26]>C(Cl)Cl>[CH3:17][N:18]1[C:23]([O:7][C:3]2[CH:4]=[N:5][CH:6]=[CH:1][CH:2]=2)=[N:22][C:21]([CH3:25])=[N:20][S:19]1(=[O:27])=[O:26]

参加物

5

反応物 3

HCID 7415N,N-DimethylcyclohexylamineHCID 79713-HydroxypyridineHCID 1588652H-1,2,4,6-Thiatriazine, 3-chloro-2,5-dimethyl-, 1,1-dioxide

生成物 1

HCID 133042862,5-Dimethyl-3-[(pyridin-3-yl)oxy]-1lambda~6~,2,4,6-thiatriazine-1,1(2H)-dione収率 68.6%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

反応条件

温度
25 °C

実験手順

17.1 parts of β-hydroxypyridine in 120 parts of methylene chloride and 19.1 parts of N,N-dimethylcyclohexylamine are introduced simultaneously, via 2 feeds, in the course of 15 minutes and at 15°-20° C., into a stirred solution of 29.3 parts of 2,5-dimethyl-3-chloro-2H-1,2,4,6-thiatriazine 1,1-dioxide in 150 parts of methylene chloride. The mixture is stirred for one hour at 25° C., after which the precipitate is filtered off under suction and the filtrate is washed with water and with dilute sodium carbonate solution, dried over magnesium sulfate, chromatographed over neutral aluminum oxide and then evaporated down under reduced pressure to give 26 parts (68.6% of theory) of 2,5-dimethyl-3-(pyrid-3-yloxy)-2H-1,2,4,6-thiatriazine 1,1-dioxide of melting point 137°-138° C. (compound No. 1).

後処理

  1. filtrationafter which the precipitate is filtered off under suction
  2. washthe filtrate is washed with water and with dilute sodium carbonate solution
  3. dry with materialdried over magnesium sulfate
  4. customchromatographed over neutral aluminum oxide
  5. customevaporated down under reduced pressure

出典と根拠

ORDレコード
ord-9792fc34d7f3477c95387079944cfcc0
出典データセット
uspto-grants-1986_04
特許番号
US04585472

反応ノート

読み込み中…