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

Diethyl Ether → HCID 178418606、化合物

HRID 1707908
ノート
印刷プレビュー

反応式

HRID 1707908 の反応式
[CH2:1]([Mg]Br)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH3:9].[O:12]1[CH2:17][CH2:16][CH2:15][CH2:14][CH:13]1[O:18][C@H:19]1[CH2:24][CH2:23][C@H:22]([C:25]2[CH:30]=[CH:29][C:28]([C:31]3C=C[C:34]([C:37]#N)=[CH:33][CH:32]=3)=[CH:27][CH:26]=2)[CH2:21][CH2:20]1.[C:39](=[O:42])([O-])[O-].[Na+].[Na+].[CH2:45](OCC)C>O1CCCC1>[O:12]1[CH2:17][CH2:16][CH2:15][CH2:14][CH:13]1[O:18][C@H:19]1[CH2:20][CH2:21][C@H:22]([C:25]2([C:39](=[O:42])[CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH3:9])[CH:30]=[CH:29][C:28]([C:31]3[CH:45]=[CH:37][CH:34]=[CH:33][CH:32]=3)=[CH:27][CH2:26]2)[CH2:23][CH2:24]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 3283Diethyl EtherHCID 10340Sodium CarbonateHCID 178418638HCID 178418638、化合物HCID 178418655HCID 178418655、化合物

生成物 1

HCID 178418606HCID 178418606、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of nonylmagnesium bromide (8.3 mmol) in 30 ml of diethyl ether was treated at 0° C. with a solution of 1.5 g of trans-4-(4'-cyano-4-biphenylyl)cyclohexyl tetrahydropyranyl ether in 15 ml of tetrahydrofuran. The reaction mixture was heated at slight reflux overnight and then treated with dilute sodium carbonate solution. The organic phase was separated and the aqueous phase was back-extracted three times with 50 ml of diethyl ether each time. The combined organic phases were washed once with dilute sodium carbonate solution and twice with water and then dried over magnesium sulfate, filtered and concentrated. The residue was purified by chromatography on silica gel with toluene/ethyl acetate (vol. 9;1). The trans-4-(4-decanoyl-4-biphenylyl)cyclohexyl tetrahydropyranyl ether (1.8 g) obtained was used in the next step without further purification.

後処理

  1. temperatureThe reaction mixture was heated
  2. temperatureat slight reflux overnight
  3. customThe organic phase was separated
  4. extractionthe aqueous phase was back-extracted three times with 50 ml of diethyl ether each time
  5. washThe combined organic phases were washed once with dilute sodium carbonate solution and twice with water
  6. dry with materialdried over magnesium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated
  9. customThe residue was purified by chromatography on silica gel with toluene/ethyl acetate (vol. 9;1)

出典と根拠

ORDレコード
ord-f1d4c58ea2694a9789de0df7ec4a8405
出典データセット
uspto-grants-1994_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05356563

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