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Sodium Hydroxide → 3-Propyl-2lambda~6~-pyrido[2,3-c][1,2,6]thiadiazine-2,2,4(1H,3H)-trione

HRID 597751
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HRID 597751 반응식
[CH2:1]([NH:4][S:5]([NH:8][C:9]1[C:14]([C:15]([O:17]C)=O)=[CH:13][CH:12]=[CH:11][N:10]=1)(=[O:7])=[O:6])[CH2:2][CH3:3].[OH-].[Na+]>O>[CH2:1]([N:4]1[S:5](=[O:7])(=[O:6])[NH:8][C:9]2[N:10]=[CH:11][CH:12]=[CH:13][C:14]=2[C:15]1=[O:17])[CH2:2][CH3:3]
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참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 22756776HCID 22756776, 화합물

생성물 1

HCID 227567853-Propyl-2lambda~6~-pyrido[2,3-c][1,2,6]thiadiazine-2,2,4(1H,3H)-trione

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Methyl 2-(((n-propylamino)sulfonyl)amino)-3-pyridinecarboxylate (15.7 grams; 0.057 mole), 95 ml of water and 10.5 ml of 50 percent aqueous sodium hydroxide were mixed and the resulting reaction mixture stirred for about one and one-fourth hours at ambient temperatures. The reaction mixture was extracted with two 50 ml portions of methylene chloride and one 50 ml portion of ether to remove impurities. The aqueous layer was separated from the organic layer and acidified to a pH of about 4.5 with concentrated hydrochloric acid. The solution was filtered and the filtrate acidified to a pH of about 1. The resulting product precipitate was recovered by filtration, dissolved in acetone and the solution filtered and dried with magnesium sulfate. The mixture was again filtered and the filtrate reduced in vacuo to obtain the title compound as a yellow powder having a melting point of 208° C.-210° C.

후처리

  1. customthe resulting reaction mixture
  2. extractionThe reaction mixture was extracted with two 50 ml portions of methylene chloride and one 50 ml portion of ether
  3. customto remove impurities
  4. customThe aqueous layer was separated from the organic layer
  5. filtrationThe solution was filtered
  6. filtrationThe resulting product precipitate was recovered by filtration
  7. dissolutiondissolved in acetone
  8. filtrationthe solution filtered
  9. dry with materialdried with magnesium sulfate
  10. filtrationThe mixture was again filtered

출처 및 근거

ORD 기록
ord-6f77211710804813bf957eef5d322a0f
출처 데이터셋
uspto-grants-1977_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04014888

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