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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 1439273
ノート
印刷プレビュー

反応式

HRID 1439273 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 22756776HCID 22756776、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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°-210° C.

後処理

  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

出典と根拠

ORDレコード
ord-84f2cb950ba94523973297d78ed9c56f
出典データセット
uspto-grants-1977_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04058533

反応ノート

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