ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Oxalyl chloride → 5-(2,4-Diisobutoxybenzoyl)-2-isobutoxyphenyl acetate

HRID 2249635
ノート
印刷プレビュー

反応式

HRID 2249635 の反応式
[C:1]([O:4][C:5]1[CH:6]=[C:7]([CH:11]=[CH:12][C:13]=1[O:14][CH2:15][CH:16]([CH3:18])[CH3:17])[C:8]([OH:10])=O)(=[O:3])[CH3:2].C(Cl)(=O)C(Cl)=O.[Cl-].[Al+3].[Cl-].[Cl-].[CH2:29]([O:33][C:34]1[CH:39]=[CH:38][CH:37]=[C:36]([O:40][CH2:41][CH:42]([CH3:44])[CH3:43])[CH:35]=1)[CH:30]([CH3:32])[CH3:31]>C(Cl)Cl.CN(C)C=O>[C:1]([O:4][C:5]1[CH:6]=[C:7]([C:8](=[O:10])[C:39]2[CH:38]=[CH:37][C:36]([O:40][CH2:41][CH:42]([CH3:44])[CH3:43])=[CH:35][C:34]=2[O:33][CH2:29][CH:30]([CH3:32])[CH3:31])[CH:11]=[CH:12][C:13]=1[O:14][CH2:15][CH:16]([CH3:18])[CH3:17])(=[O:3])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 65578Oxalyl chlorideHCID 6451240Aluminum(III) ChlorideHCID 130875651,3-DiisobutoxybenzeneHCID 178164733-(Acetyloxy)-4-isobutoxybenzoic acid

生成物 1

HCID 178164575-(2,4-Diisobutoxybenzoyl)-2-isobutoxyphenyl acetate収率 68.5%

試薬・触媒・溶媒 2

HCID 6228
Dimethylformamide
溶媒
HCID 6344Dichloromethane溶媒2 回

実験手順

In 10 ml of methylene chloride is dissolved 1.00 g of 3-(acetyloxy)-4-isobutoxybenzoic acid. After adding 0.41 ml of oxalyl chloride and 20 μl of N,N-dimethylformamide successively at ambient temperature, the mixture thus obtained is stirred at ambient temperature for one hour. Then, 1.06 g of aluminum chloride and 1.15 g of 1,3-diisobutoxybenzene are successively added at 5-10° C., and the mixture is stirred at the same temperature as above for one hour. The reaction mixture is added to a mixture of methylene chloride and ice water, and the organic layer is separated. The organic layer is successively washed with water and saturated aqueous solution of sodium chloride and dried over anhydrous magnesium sulfate, and the solvent is distilled off under reduced pressure. The residue thus obtained is purified by silica gel column chromatography [eluent; n-hexane:ethyl acetate=5:1] to obtain 1.24 g of 5-(2,4-diisobutoxybenzoyl)-2-isobutoxyphenyl acetate as a yellow oily product.

後処理

  1. customthe mixture thus obtained
  2. stirringthe mixture is stirred at the same temperature as above for one hour
  3. customthe organic layer is separated
  4. washThe organic layer is successively washed with water and saturated aqueous solution of sodium chloride
  5. dry with materialdried over anhydrous magnesium sulfate
  6. distillationthe solvent is distilled off under reduced pressure
  7. customThe residue thus obtained
  8. customis purified by silica gel column chromatography [eluent; n-hexane:ethyl acetate=5:1]

出典と根拠

ORDレコード
ord-ea17877cfbc14e52943175709ae06e5a
出典データセット
uspto-grants-2008_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07314888B1

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート