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

Tetrahydrofuran → HCID 22915773、化合物

HRID 1376299
ノート
印刷プレビュー

反応式

HRID 1376299 の反応式
[Br-].[O:2]1[CH2:7][CH2:6][CH2:5][O:4][CH:3]1[CH2:8][CH2:9][P+](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.O1CCCC1.CC(C)([O-])C.[K+].[F:40][C:41]1[CH:42]=[C:43]([CH:52]2[CH2:57][CH2:56][C:55](=O)[CH2:54][CH2:53]2)[CH:44]=[CH:45][C:46]=1[O:47][C:48]([F:51])([F:50])[F:49]>CCOCC>[O:4]1[CH2:5][CH2:6][CH2:7][O:2][CH:3]1[CH2:8][CH:9]=[C:55]1[CH2:54][CH2:53][CH:52]([C:43]2[CH:44]=[CH:45][C:46]([O:47][C:48]([F:49])([F:51])[F:50])=[C:41]([F:40])[CH:42]=2)[CH2:57][CH2:56]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 8028Tetrahydrofuran2 回HCID 27241682-(1,3-Dioxan-2-yl)ethyltriphenylphosphonium bromideHCID 21993296HCID 21993296、化合物HCID 23665647Potassium tert-butoxide

生成物 1

HCID 22915773HCID 22915773、化合物

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether
溶媒

実験手順

Into a three-necked flask equipped with a dropping funnel, a three-way cook and a thermometer was placed 2-(1,3-dioxan-2-yl)ethyltriphenylphosphonium bromide (9.1 g, 20 mmols), followed by adding tetrahydrofuran (100 ml), suspending, stirring under ice cooling till the liquid temperature reached 10° C. The resulting reaction mixture was added potassium t-butoxide (2.2 g, 20 mmols) followed by elevating the temperature up to room temperature under ice cooling for one hour, stirring for one hour, dropwise adding a tetrahydrofuran (50 ml) solution of 4-(3-fluoro-4-trifluoromethoxyphenyl)cyclohexanone (5.5 g, 20 mmols) over 30 minutes from the dropping funnel, further stirring the reaction mixture for 5 hours after completion of the dropwise addition, adding ether (100 ml), allowing to stand for one hour, filtering off deposited insoluble substance, concentrating the filtrate under reduced pressure, and isolating and purifying the resulting pale brown oil by means of silica gel column chromatography, to obtain 1-(2-(1,3-dioxan-2-yl)ethylidene)-4-(3-fluoro-4-trifluoromethoxyphenyl)cyclohexane.

後処理

  1. customInto a three-necked flask equipped with a dropping funnel
  2. customreached 10° C
  3. customThe resulting reaction mixture
  4. customup to room temperature
  5. customfor one hour
  6. stirringstirring for one hour
  7. stirringfurther stirring the reaction mixture for 5 hours
  8. additionafter completion of the dropwise addition
  9. filtrationfiltering off
  10. concentrationconcentrating the filtrate under reduced pressure
  11. customisolating
  12. custompurifying the resulting pale brown oil by means of silica gel column chromatography

出典と根拠

ORDレコード
ord-a4ab46ba8619492eb98683363652c4eb
出典データセット
uspto-grants-1997_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05662830

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