1,4-Dioxane hydrochloride → HCID 23117571、化合物

HRID 1178324ノート

反応式

HRID 1178324 の反応式
Cl.O1CCOCC1.C(=[N:15][C:16]([C:25]1[CH:30]=[CH:29][C:28]([Cl:31])=[C:27]([Cl:32])[CH:26]=1)([CH2:22][CH:23]=[CH2:24])[C:17]([O:19][CH2:20][CH3:21])=[O:18])C1C=CC=CC=1>O>[NH2:15][C:16]([C:25]1[CH:30]=[CH:29][C:28]([Cl:31])=[C:27]([Cl:32])[CH:26]=1)([CH2:22][CH:23]=[CH2:24])[C:17]([O:19][CH2:20][CH3:21])=[O:18]

参加物

4

反応物 2

HCID 204431481,4-Dioxane hydrochlorideHCID 23117635HCID 23117635、化合物

生成物 1

HCID 23117571HCID 23117571、化合物収率 58.2%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

4N HCl-1,4-dioxane (308 mL) and water (65 mL) were added to ethyl 2-(benzylidene-amino)-2-(3,4-dichlorophenyl)-4-pentenoate (518 g), followed by stirring at room temperature for 3 hours. The reaction mixture was concentrated under reduced pressure. Water (1 L) and 1N aqueous hydrochloric acid (500 mL) were added to the residue, and the mixture was washed with diisopropyl ether (500 mL) three times. 25% Aqueous sodium hydroxide (250 mL) was added to the aqueous layer to adjust the pH to 9. The resultant mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine and dried over sodium sulfate anhydrate. The solvent was removed under reduced pressure, to thereby give the title compound (231 g). The title compound was used in the next step without further purification.

後処理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. additionWater (1 L) and 1N aqueous hydrochloric acid (500 mL) were added to the residue
  3. washthe mixture was washed with diisopropyl ether (500 mL) three times
  4. addition25% Aqueous sodium hydroxide (250 mL) was added to the aqueous layer
  5. extractionThe resultant mixture was extracted with ethyl acetate
  6. washThe organic layer was washed with saturated brine
  7. dry with materialdried over sodium sulfate anhydrate
  8. customThe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-938c0408a0dd441a85a3bd72c8b54a4d
出典データセット
uspto-grants-2007_10
特許番号
US07276511B2

反応ノート

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