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

HRID 1381059노트

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HRID 1381059 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

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온도
25 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-9792fc34d7f3477c95387079944cfcc0
출처 데이터셋
uspto-grants-1986_04
특허 번호
US04585472

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