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Sodium Hydroxide → 2,2,7-Trimethyl-1,3-dioxolo-[4,5-g]-quinoxaline-6-carboxylic acid, 1,1-dimethylethyl ester

HRID 486279
ノート
印刷プレビュー

反応式

HRID 486279 の反応式
[NH2:1][C:2]1[C:12]([NH2:13])=[CH:11][C:5]2[O:6][C:7]([CH3:10])([CH3:9])[O:8][C:4]=2[CH:3]=1.C1(N)C(F)=C(F)C(F)=C(N)C=1F.Cl.Cl.[OH-].[Na+].[C:30]([O:34][C:35](=[O:41])[C:36](=O)[C:37](=O)[CH3:38])([CH3:33])([CH3:32])[CH3:31]>O.O1CCCC1>[CH3:9][C:7]1([CH3:10])[O:6][C:5]2=[CH:11][C:12]3[N:13]=[C:37]([CH3:38])[C:36]([C:35]([O:34][C:30]([CH3:33])([CH3:32])[CH3:31])=[O:41])=[N:1][C:2]=3[CH:3]=[C:4]2[O:8]1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 14798Sodium HydroxideHCID 149026Tetrafluoro-m-phenylenediamine dihydrochlorideHCID 10986731Tert-butyl 2,3-dioxobutanoateHCID 13343758HCID 13343758、化合物

生成物 1

HCID 540074732,2,7-Trimethyl-1,3-dioxolo-[4,5-g]-quinoxaline-6-carboxylic acid, 1,1-dimethylethyl ester

試薬・触媒・溶媒 2

HCID 962
Water
溶媒
HCID 8028Tetrahydrofuran溶媒

実験手順

[5,6-diamino-2,2-dimethyl-1,3-benzodioxole; dihydrochloride salt] (U.S. Pat. No. 4,904,775, Example 3D) (6.8 g, 0.02 mmol) was dissolved in a mixture of 25 ml water and 10 ml tetrahydrofuran and the pH of the solution was adjusted to 5.5 by the addition of 2N NaOH. After addition of the compound from Example 1 (3.8 g; 0.02 mol) the mixture was refluxed for 2 hours, concentrated in vacuo to remove the organic solvent tetrahydrofuran and then extracted with ethyl acetate. The combined organic phases were washed with brine, dried (Na2SO4) and then evaporated in vacuo to leave an oil which crystallized by the addition of petroleum ether. M.P. 104°-105° C.; yield 5.2 g (82%).

後処理

  1. temperaturewas refluxed for 2 hours
  2. concentrationconcentrated in vacuo
  3. customto remove the organic solvent tetrahydrofuran
  4. extractionextracted with ethyl acetate
  5. washThe combined organic phases were washed with brine
  6. dry with materialdried (Na2SO4)
  7. customevaporated in vacuo
  8. customto leave an oil which
  9. customcrystallized by the addition of petroleum ether

出典と根拠

ORDレコード
ord-65385544a6d347aab4fa622640562edf
出典データセット
uspto-grants-1994_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05290929

反応ノート

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