Ibuprofen, (+-)- → Phthalidyl 2-(4-isobutylphenyl)propionate

HRID 371108

反応式

HRID 371108 の反応式
[CH2:1]([C:5]1[CH:10]=[CH:9][C:8]([CH:11]([CH3:15])[C:12]([OH:14])=[O:13])=[CH:7][CH:6]=1)[CH:2]([CH3:4])[CH3:3].Br[CH:17]1[C:26]2[C:21](=[CH:22][CH:23]=[CH:24][CH:25]=2)[C:19](=[O:20])[O:18]1>C(Cl)(Cl)Cl.C(N(CC)CC)C>[CH2:1]([C:5]1[CH:6]=[CH:7][C:8]([CH:11]([CH3:15])[C:12]([O:14][CH:17]2[C:26]3[C:21](=[CH:22][CH:23]=[CH:24][CH:25]=3)[C:19](=[O:20])[O:18]2)=[O:13])=[CH:9][CH:10]=1)[CH:2]([CH3:4])[CH3:3]

参加物

5

反応物 2

HCID 3672Ibuprofen, (+-)-HCID 962181(3H)-Isobenzofuranone, 3-bromo-

生成物 1

HCID 12769702Phthalidyl 2-(4-isobutylphenyl)propionate収率 82.2%

試薬・触媒・溶媒 2

HCID 6212Chloroform溶媒2 回HCID 8471Triethylamine溶媒

実験手順

To a solution of 6.2 g of 2-(4-isobutylphenyl)propionic acid in 30 ml of chloroform and 3.4 g of triethylamine, a solution of 6.2 g of 3-bromophthalide in 20 ml of chloroform is added. The solution thus obtained is stirred 24 hours at room temperature (about +22° C.), the organic phase is washed with an aqueous solution of sodium bicarbonate, then with water and finally it is dried on anhydrous sodium sulfate and evaporated to dryness. The residue, crystallized from petroleum ether, yields 8.1 g of phthalidyl 2-(4-isobutylphenyl)propionate; m.p. 62°-65° C. IR: 1795 and 1780 cm1

後処理

  1. customThe solution thus obtained
  2. washthe organic phase is washed with an aqueous solution of sodium bicarbonate
  3. dry with materialwith water and finally it is dried on anhydrous sodium sulfate
  4. customevaporated to dryness
  5. customThe residue, crystallized from petroleum ether

出典と根拠

ORDレコード
ord-becd6a5b7db84e83858dbfd9caf14c78
出典データセット
uspto-grants-1985_07
特許番号
US04529737

関連ノート

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