Hydrochloric Acid → 4-[(5,6,6a,7,8,9-Hexahydro-4H-2-phenalenyl)carbamoyl]benzoic acid

HRID 1517489ノート

反応式

HRID 1517489 の反応式
[CH:1]1[C:12]2=[C:13]3[CH:8]([CH2:9][CH2:10][CH2:11]2)[CH2:7][CH2:6][CH2:5][C:4]3=[CH:3][C:2]=1[NH:14][C:15]([C:17]1[CH:26]=[CH:25][C:20]([C:21]([O:23]C)=[O:22])=[CH:19][CH:18]=1)=[O:16].[OH-].[Na+].Cl>C(O)C>[CH:3]1[C:4]2=[C:13]3[CH:8]([CH2:7][CH2:6][CH2:5]2)[CH2:9][CH2:10][CH2:11][C:12]3=[CH:1][C:2]=1[NH:14][C:15]([C:17]1[CH:18]=[CH:19][C:20]([C:21]([OH:23])=[O:22])=[CH:25][CH:26]=1)=[O:16]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 67391601HCID 67391601、化合物

生成物 1

HCID 673911074-[(5,6,6a,7,8,9-Hexahydro-4H-2-phenalenyl)carbamoyl]benzoic acid収率 90%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A suspension of methyl 4-[(5,6,6a,7,8,9-hexahydro-4H-2-phenalenyl)carbamoyl]benzoate (0.093 g) in ethanol (10 ml) was added with 2 N aqueous sodium hydroxide (3 ml), and the mixture was stirred at room temperature for 3 hours. The reaction mixture was made acidic with 2 N aqueous hydrochloric acid, and extracted with chloroform. The organic layer was washed with saturated brine, and dried over anhydrous sodium sulfate. The organic layer was concentrated under reduced pressure, and the resulting residue was recrystallized from ethyl acetate-n-hexane to obtain the title compound (0.080 g, yield: 90%) as colorless prisms (melting point: 283-284° C.).

後処理

  1. extractionextracted with chloroform
  2. washThe organic layer was washed with saturated brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationThe organic layer was concentrated under reduced pressure
  5. customthe resulting residue was recrystallized from ethyl acetate-n-hexane

出典と根拠

ORDレコード
ord-277e1b9590af4bf0a69f9eab9887cdbe
出典データセット
uspto-grants-2012_07
特許番号
US08232300B2

反応ノート

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