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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
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HRID 2210461 반응식
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]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

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

생성물 1

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

시약·촉매·용매 2

HCID 962Water용매HCID 6342Acetonitrile
용매

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온도
50 °C

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-595e0b7f26e54779ba8346dc51222586
출처 데이터셋
uspto-grants-1995_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05459138

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