Benzene → HCID 25189876、化合物

HRID 1517501ノート

反応式

HRID 1517501 の反応式
[CH3:1][C:2]12[C:14]3[C:6](=[CH:7][C:8]([NH2:15])=[CH:9][C:10]=3[CH2:11][CH2:12][CH2:13]1)[CH2:5][CH2:4][CH2:3]2.C1C=CC=CC=1.Cl[S:23]([C:26]1[CH:34]=[CH:33][C:29]([C:30]([OH:32])=[O:31])=[CH:28][CH:27]=1)(=[O:25])=[O:24].Cl>N1C=CC=CC=1.CN(C)C1C=CN=CC=1>[CH3:1][C:2]12[C:14]3[C:6](=[CH:7][C:8]([NH:15][S:23]([C:26]4[CH:27]=[CH:28][C:29]([C:30]([OH:32])=[O:31])=[CH:33][CH:34]=4)(=[O:25])=[O:24])=[CH:9][C:10]=3[CH2:11][CH2:12][CH2:13]1)[CH2:5][CH2:4][CH2:3]2

参加物

7

反応物 4

HCID 241BenzeneHCID 313Hydrochloric AcidHCID 823854-(Chlorosulfonyl)benzoic acidHCID 58420583HCID 58420583、化合物

生成物 1

HCID 25189876HCID 25189876、化合物収率 57.4%

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 1049Pyridine溶媒

実験手順

6a-Methyl-5,6,6a,7,8,9-hexahydro-4H-2-phenalenylamine (0.100 g) was dissolved in pyridine (5 ml) and anhydrous benzene (2 ml), the solution was added with 4-chlorosulfonylbenzoic acid (0.115 g) and 4-dimethylaminopyridine (one pellet), and the mixture was stirred overnight at room temperature. The reaction mixture was added with 2 N aqueous hydrochloric acid and thereby made acidic, and the mixture was 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 (0.110 g, yield: 57%) as colorless needles (melting point: 215-217° C.).

後処理

  1. extractionmade acidic, and the mixture was extracted 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-a35b14332ec742f9a002852f59e4d4a9
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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