2-(8-Iodooctyl)-4,5,6,7-tetramethoxyindan → HCID 18348600、化合物

HRID 2268475

反応式

HRID 2268475 の反応式
I[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH:10]1[CH2:18][C:17]2[C:12](=[C:13]([O:25][CH3:26])[C:14]([O:23][CH3:24])=[C:15]([O:21][CH3:22])[C:16]=2[O:19][CH3:20])[CH2:11]1.[C:27]1(=[O:37])[NH:31][C:30](=[O:32])[C:29]2=[CH:33][CH:34]=[CH:35][CH:36]=[C:28]12.[K]>CN(C=O)C.C(OCC)(=O)C>[CH3:26][O:25][C:13]1[C:14]([O:23][CH3:24])=[C:15]([O:21][CH3:22])[C:16]([O:19][CH3:20])=[C:17]2[C:12]=1[CH2:11][CH:10]([CH2:9][CH2:8][CH2:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2][N:31]1[C:30](=[O:32])[C:29]3=[CH:33][CH:34]=[CH:35][CH:36]=[C:28]3[C:27]1=[O:37])[CH2:18]2

参加物

5

反応物 2

HCID 183485412-(8-Iodooctyl)-4,5,6,7-tetramethoxyindanHCID 24194345Phthalimide potassium salt

生成物 1

HCID 18348600HCID 18348600、化合物収率 84.5%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of 2-(8-iodooctyl)-4,5,6,7-tetramethoxyindan (1.98 g) in DMF (10 ml) was dropwise added potassium phthalimide (924 mg). After being stirred at room temperature for 12 hr, the reaction mixture was diluted with ethyl acetate. The organic layer was washed with water and saturated aqueous sodium chloride and dried. The solvent was removed in vacuo and the residue was purified by alumina column chromatography (hexane to hexane:ethyl acetate=10:1) and then recrystallized from hexane gave the entitled compound (1.74 g) as crystals.

後処理

  1. washThe organic layer was washed with water and saturated aqueous sodium chloride
  2. customdried
  3. customThe solvent was removed in vacuo
  4. customthe residue was purified by alumina column chromatography (hexane to hexane:ethyl acetate=10:1)
  5. customrecrystallized from hexane

出典と根拠

ORDレコード
ord-27ca368188ec4fc688f41f82c13cf516
出典データセット
uspto-grants-2001_12
特許番号
US06326369B1

関連ノート

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