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Dimethyl Sulfate → 1-Methyl-3-(1-methylethyl)-pyrido(2,3-c)(1,2,6)-thiadiazin-4(3H)-one-2,2-dioxide

HRID 866470
ノート
印刷プレビュー

反応式

HRID 866470 の反応式
[CH3:1][CH:2]([N:4]1[S:9](=[O:11])(=[O:10])[NH:8][C:7]2[N:12]=[CH:13][CH:14]=[CH:15][C:6]=2[C:5]1=[O:16])[CH3:3].[H-].[Na+].S(OC)(O[CH3:23])(=O)=O>COCCOCCOC>[CH3:23][N:8]1[C:7]2[N:12]=[CH:13][CH:14]=[CH:15][C:6]=2[C:5](=[O:16])[N:4]([CH:2]([CH3:1])[CH3:3])[S:9]1(=[O:10])=[O:11]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6497Dimethyl SulfateHCID 24758Sodium hydrideHCID 136092433-(1-Methylethyl)pyrido(2,3-c) (1,2,6)thiadiazin-4(3H)-one-2,2-dioxide

生成物 1

HCID 227567831-Methyl-3-(1-methylethyl)-pyrido(2,3-c)(1,2,6)-thiadiazin-4(3H)-one-2,2-dioxide

試薬・触媒・溶媒 1

HCID 8150Diglyme溶媒

実験手順

3-(1-Methylethyl)pyrido(2,3-c)(1,2,6)thiadiazin-4(3H)-one-2,2-dioxide (5.0 grams; 0.0208 mole) was mixed with 50 ml of diethylene glycol dimethyl ether. The system was flushed with nitrogen and sodium hydride (1.0 gram; 0.02 mole), previously washed with n-hexane, was added portionwise to the reaction mixture. After the effervescence of hydrogen ceased, 2.2 ml of dimethyl sulfate (0.023 mole, 1.33g/ml) was added and the reaction mixture heated at reflux temperatures for a period of 4 hours. During the reaction, the color of the reaction mixture changed from light yellow to deep red and gradually back to yellow.

後処理

  1. washpreviously washed with n-hexane
  2. additionwas added portionwise to the reaction mixture
  3. temperaturethe reaction mixture heated
  4. temperatureat reflux temperatures for a period of 4 hours
  5. customDuring the reaction

出典と根拠

ORDレコード
ord-5d7b25d6acff43bda768d2b132933521
出典データセット
uspto-grants-1978_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04098792

反応ノート

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