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Hydrochloric Acid → 2-(7-Chloro-2,3-dihydro-2-methyl-4-benzofuranyl)-2,3,4,5-tetrahydro-3,5-dioxo-1,2,4-triazine-6-carboxylic acid

HRID 1709120
ノート
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反応式

HRID 1709120 の反応式
ClC1[C:10]2OC(C)C[C:6]=2[C:5]([N:12]2[C:17](=[O:18])[NH:16][C:15](=[O:19])C(C#N)=[N:13]2)=[CH:4][CH:3]=1.O1[CH2:27][CH2:26][O:25][CH2:24][CH2:23]1.[ClH:28].[C:29]([O:32]CC)(=[O:31])[CH3:30]>>[Cl:28][C:27]1[C:26]2[O:25][CH:24]([CH3:23])[CH2:10][C:6]=2[C:5]([N:12]2[C:17](=[O:18])[NH:16][C:15](=[O:19])[C:30]([C:29]([OH:32])=[O:31])=[N:13]2)=[CH:4][CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 4

HCID 313Hydrochloric Acid2 回HCID 8857Ethyl AcetateHCID 312751,4-DioxaneHCID 542357422-(7-Chloro-2,3-dihydro-2-methyl-4-benzofuranyl)-2,3,4,5-tetrahydro-3,5-dioxo-1,2,4-triazine-6-carbonitrile

生成物 1

HCID 541828772-(7-Chloro-2,3-dihydro-2-methyl-4-benzofuranyl)-2,3,4,5-tetrahydro-3,5-dioxo-1,2,4-triazine-6-carboxylic acid

実験手順

A mixture of 9.0 g of 32C, 150 mL of p-dioxane and 100 mL of 6N hydrochloric acid was stirred at reflux temperature overnight. Then 20 mL of 12N hydrochloric acid was added and the mixture was stirred at reflux temperature for 2 hours, and stripped of solvent. The residue was dissolved in ethyl acetate, the solution was washed with water, then brine, dried (MgSO4) and stripped of solvent. The residue was recrystallized from ethyl acetate/petroleum ether to give 2-(7-chloro-2,3-dihydro-2-methyl-4-benzofuranyl)-2,3,4,5-tetrahydro-3,5-dioxo-1,2,4-triazine-6-carboxylic acid (32D), as an amber solid, m.p.: 235°-236° C. (with decomposition).

後処理

  1. temperatureat reflux temperature overnight
  2. stirringthe mixture was stirred
  3. temperatureat reflux temperature for 2 hours
  4. washthe solution was washed with water
  5. dry with materialbrine, dried (MgSO4)
  6. customThe residue was recrystallized from ethyl acetate/petroleum ether

出典と根拠

ORDレコード
ord-9cd1a72c81b645a18bfe1485ff66021a
出典データセット
uspto-grants-1990_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04948418

反応ノート

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