Hydrochloric Acid → HCID 67391601、化合物

HRID 1517488ノート

反応式

HRID 1517488 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[NH2:14].[Cl-].[C:16]([O:27][CH3:28])(=[O:26])[C:17]1[CH:25]=[CH:24][C:20]([C:21]([O-])=[O:22])=[CH:19][CH:18]=1.Cl>C1C=CC=CC=1.N1C=CC=CC=1>[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:21]([C:20]1[CH:24]=[CH:25][C:17]([C:16]([O:27][CH3:28])=[O:26])=[CH:18][CH:19]=1)=[O:22]

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 22493623Monomethyl terephthalate chlorideHCID 58420580HCID 58420580、化合物

生成物 1

HCID 67391601HCID 67391601、化合物収率 95%

試薬・触媒・溶媒 2

HCID 241Benzene溶媒HCID 1049Pyridine溶媒

実験手順

A solution of 5,6,6a,7,8,9-hexahydro-4H-2-phenalenylamine (0.260 g) in anhydrous benzene (10 ml) and pyridine (3 ml) was added with monomethyl terephthalate chloride (0.304 g), and the mixture was stirred at room temperature for 3 hours. The reaction mixture was added with 2 N aqueous hydrochloric acid and thereby made acidic, and the mixture was extracted with ethyl acetate. The organic layer was washed successively with water, 10% aqueous sodium carbonate, water and saturated brine, and then dried over anhydrous sodium sulfate. The organic layer was concentrated under reduced pressure, and the resulting residue was recrystallized from chloroform-n-hexane to obtain the title compound (0.460 g, yield: 95%) as colorless needles (melting point: 217-218° C.).

後処理

  1. extractionmade acidic, and the mixture was extracted with ethyl acetate
  2. washThe organic layer was washed successively with water, 10% aqueous sodium carbonate, water and 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 chloroform-n-hexane

出典と根拠

ORDレコード
ord-a8e4fdc8f05e41f19d300971ad671318
出典データセット
uspto-grants-2012_07
特許番号
US08232300B2

反応ノート

読み込み中…