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

Ammonium Chloride → tert-Butyl 4-(1-hydroxypropyl)benzoate

HRID 742309
ノート
印刷プレビュー

反応式

HRID 742309 の反応式
[CH:1]([C:3]1[CH:15]=[CH:14][C:6]([C:7]([O:9][C:10]([CH3:13])([CH3:12])[CH3:11])=[O:8])=[CH:5][CH:4]=1)=[O:2].[CH2:16]([Mg]Br)[CH3:17].[Cl-].[NH4+]>CCOCC>[OH:2][CH:1]([C:3]1[CH:15]=[CH:14][C:6]([C:7]([O:9][C:10]([CH3:11])([CH3:12])[CH3:13])=[O:8])=[CH:5][CH:4]=1)[CH2:16][CH3:17]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 25517Ammonium ChlorideHCID 2751588Tert-butyl 4-formylbenzoateHCID 178418443HCID 178418443、化合物

生成物 1

HCID 21473763tert-Butyl 4-(1-hydroxypropyl)benzoate

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

t-Butyl p-formylbenzoate (20 g, 97 mmol) was dissolved in ether (300 ml), followed by the dropwise addition of ethylmagnesium bromide (3M ethereal solution, 33 ml) under cooling with ice. The obtained mixture was stirred to complete a reaction. The reaction mixture was poured into a saturated aqueous solution of ammonium chloride and the obtained mixture was extracted with ether. The organic phase was distilled to remove the solvent and the obtained residue was subjected to silica gel column chromatography and eluted with a solvent (ethyl acetate/hexane=1:4) to give 22.3 g of t-butyl 4-(1-hydroxypropyl)benzoate. This product was dissolved in petroleum ether (500 ml), followed by the addition of active manganese dioxide (165 g). The obtained mixture was heated under reflux for 30 hours to complete a reaction. The reaction mixture was filtered and the filtrate was concentrated to give 21.1 g of t-butyl 4-propionylbenzoate.

後処理

  1. temperatureunder cooling with ice
  2. customa reaction
  3. extractionthe obtained mixture was extracted with ether
  4. distillationThe organic phase was distilled
  5. customto remove the solvent
  6. washeluted with a solvent (ethyl acetate/hexane=1:4)

出典と根拠

ORDレコード
ord-0510194de25a419da8e567c741c45216
出典データセット
uspto-grants-1996_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05554615

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