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Methyl iodide → 2H-Pyrido[3,2-e]-1,2,4-thiadiazine,3,4-dihydro-2-methyl-,1,1-dioxide(9CI)

HRID 2210461
ノート
印刷プレビュー

反応式

HRID 2210461 の反応式
C(=O)([O-])[O-].[K+].[K+].I[CH3:8].[S:9]1(=[O:20])(=[O:19])[C:14]2[N:15]=[CH:16][CH:17]=[CH:18][C:13]=2[NH:12][CH2:11][NH:10]1>C(#N)C.O>[CH3:8][N:10]1[CH2:11][NH:12][C:13]2[CH:18]=[CH:17][CH:16]=[N:15][C:14]=2[S:9]1(=[O:20])=[O:19]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 108213802,3-DIHYDRO-4H-PYRIDO[3,2-e] [1,2,4]THIADIAZINE 1,1-DIOXIDE

生成物 1

HCID 104882192H-Pyrido[3,2-e]-1,2,4-thiadiazine,3,4-dihydro-2-methyl-,1,1-dioxide(9CI)

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6342Acetonitrile
溶媒

反応条件

温度
50 °C

実験手順

0.52 g of potassium carbonate and 0.94 g of iodomethane are added to a solution of 0.25 g of 2,3- dihydro-4H-pyrido[3,2-e][1,2,4]thiadiazine 1,1-dioxide (Example 1) in 10 cm3 of acetonitrile. The suspension is heated at 50° C. for 3 hours. The acetonitrile is then removed by evaporation under partial vacuum and the residue obtained is taken up in 10 cm3 of water. The suspension is extracted with chloroform (5 times 100 cm3). The extraction solvent is dried over MgSO4 and then concentrated to dryness. The solid obtained is purified by chromatography on a silica column (elution solvent: 1/9 MeOH/CHCl3).

後処理

  1. customThe acetonitrile is then removed by evaporation under partial vacuum
  2. customthe residue obtained
  3. extractionThe suspension is extracted with chloroform (5 times 100 cm3)
  4. dry with materialThe extraction solvent is dried over MgSO4
  5. concentrationconcentrated to dryness
  6. customThe solid obtained
  7. customis purified by chromatography on a silica column (elution solvent: 1/9 MeOH/CHCl3)

出典と根拠

ORDレコード
ord-595e0b7f26e54779ba8346dc51222586
出典データセット
uspto-grants-1995_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05459138

反応ノート

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