HCID 14770843、化合物 → HCID 14770834、化合物

HRID 1090381ノート

反応式

HRID 1090381 の反応式
[Br:1][C:2]1[CH:7]=[C:6]([F:8])[C:5]([CH:9]2[CH2:13][CH2:12][CH:11](Cl)[CH2:10]2)=[CH:4][C:3]=1[F:15].[C:16]1(=[O:26])[NH:20][C:19](=[O:21])[C:18]2=[CH:22][CH:23]=[CH:24][CH:25]=[C:17]12.[K]>CN(C)C=O>[Br:1][C:2]1[C:3]([F:15])=[CH:4][C:5]([CH:9]2[CH2:13][CH2:12][CH:11]([N:20]3[C:16](=[O:26])[C:17]4[C:18](=[CH:22][CH:23]=[CH:24][CH:25]=4)[C:19]3=[O:21])[CH2:10]2)=[C:6]([F:8])[CH:7]=1

参加物

4

反応物 2

HCID 14770843HCID 14770843、化合物HCID 24194345Phthalimide potassium salt

生成物 1

HCID 14770834HCID 14770834、化合物収率 90.6%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A solution of 29.6 g (0.1 mol) of 1-bromo-4-(3-chlorocyclopentyl)-2,5-difluorobenzene in 150 ml of dry dimethylformamide was treated with 19.4 g (0.105 mol) of potassium phthalimide and the resulting suspension stirred at 100° for 8 hours and room temperature overnight. The solvent was removed in vacuo, and the residue was partitioned between methylene chloride and water. The aqueous layer was reextracted with methylene chloride and the combined organic layers were washed with water, dried (MgSO4), filtered, and evaporated in vacuo to give 36.8 g of the title compound as a viscous oil which crystallized on standing and had mp 44°-47°.

後処理

  1. customThe solvent was removed in vacuo
  2. customthe residue was partitioned between methylene chloride and water
  3. washthe combined organic layers were washed with water
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. customevaporated in vacuo

出典と根拠

ORDレコード
ord-a0e178e7814f4da59c8a4b3f2afedf87
出典データセット
uspto-grants-1992_01
特許番号
US05081254

反応ノート

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