Water → 2-Cyclohexyl-5-methoxy-2H-1,2,4,6-thiatriazin-3-one-1,1-dioxide

HRID 246838ノート

反応式

HRID 246838 の反応式
C([N:5]([S:10](=[O:19])(=[O:18])[NH:11][CH:12]1[CH2:17][CH2:16][CH2:15][CH2:14][CH2:13]1)[C:6](=[NH:9])[O:7][CH3:8])(OC)=O.[H-].[Na+].O.C1C[O:26][CH2:25]C1>>[CH:12]1([N:11]2[C:25](=[O:26])[NH:9][C:6]([O:7][CH3:8])=[N:5][S:10]2(=[O:18])=[O:19])[CH2:13][CH2:14][CH2:15][CH2:16][CH2:17]1

参加物

5

反応物 4

HCID 962WaterHCID 8028Tetrahydrofuran2 回HCID 24758Sodium hydrideHCID 21269103N-Carbomethoxy-N-cyclohexylsulfamyl-O-methylisourea

生成物 1

HCID 130177642-Cyclohexyl-5-methoxy-2H-1,2,4,6-thiatriazin-3-one-1,1-dioxide

実験手順

A solution of the isourea from Step 1. above (208.9 g) in anhydrous THF (500 ml) is added dropwise to a stirred suspension of 60% sodium hydride dispersion (57.0 g) in anhydrous THF (750 ml) and the reaction mixture is refluxed for 2 hours. Distilled water (450 ml) is added dropwise to the stirred mixture which is washed with diethyl ether. 20% sulfuric acid (400 ml) is added slowly to the stirred reaction mixture, which is extracted with methylene chloride, dried, filtered, and the filtrate evaporated and dried under high vacuum yielding the desired product as a crude solid which is used in the next step without further purification.

後処理

  1. temperaturethe reaction mixture is refluxed for 2 hours
  2. washis washed with diethyl ether
  3. addition20% sulfuric acid (400 ml) is added slowly to the stirred reaction mixture, which
  4. extractionis extracted with methylene chloride
  5. customdried
  6. filtrationfiltered
  7. customthe filtrate evaporated
  8. customdried under high vacuum

出典と根拠

ORDレコード
ord-952999eb7ff04ae597e82dbb5cfa7816
出典データセット
uspto-grants-1987_11
特許番号
US04704388

反応ノート

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