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 → 2-(5-ethoxyhept-1-yl)bicyclo[3.3.0]octan-7-one 4-(5-ethoxyheptyl)hexahydro-2(1H)-pentalenone

HRID 1722363
ノート
印刷プレビュー

反応式

HRID 1722363 の反応式
[N+](=C)=[N-].CCOCC.[CH2:9]([O:11][CH:12]([CH2:26][CH3:27])[CH2:13][CH2:14][CH2:15][CH2:16][CH:17]1[CH2:24][CH2:23][CH:22]2[CH:18]1[CH2:19][C:20](=[O:25])[CH2:21]2)[CH3:10].COC(CC)CCCCC1CCC2C1CC(=O)C2>C(O)(=O)C.[Zn]>[CH2:9]([O:11][CH:12]([CH2:26][CH3:27])[CH2:13][CH2:14][CH2:15][CH2:16][CH:17]1[CH2:24][CH2:23][CH:22]2[CH:18]1[CH2:19][C:20](=[O:25])[CH2:21]2)[CH3:10].[CH2:9]([O:11][CH:12]([CH2:26][CH3:27])[CH2:13][CH2:14][CH2:15][CH2:16][CH:17]1[CH2:24][CH2:23][CH:22]2[CH:18]1[CH2:19][C:20](=[O:25])[CH2:21]2)[CH3:10]
参加物反応条件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 3283Diethyl EtherHCID 9550DiazomethaneHCID 55994CioteronelHCID 104007396-(5-Ethoxyhept-1-yl)bicyclo[3.3.0]octan-3-one

生成物 1

HCID 200287092-(5-ethoxyhept-1-yl)bicyclo[3.3.0]octan-7-one 4-(5-ethoxyheptyl)hexahydro-2(1H)-pentalenone

試薬・触媒・溶媒 2

HCID 23994
Zinc
触媒
HCID 176Acetic Acid溶媒2 回

反応条件

温度
70 °C

実験手順

After 50 minutes the excess diazomethane is neutralized with the addition of acetic acid (10 ml). The solvent is removed under vacuum leaving a clear yellow liquid. The crude product is then diluted with acetic acid (240 ml) and stirred while zinc powder (72 g, 1.10 moles) is slowly added. The reaction is heated in a 70° C. water bath for 1 hour, after which time ether (500 ml) is added and the solution filtered. The ether layer is washed with brine (100 ml) and then with a solution of saturated bicarbonate. The ether layer is separated and dried over sodium sulfate. The solvent is removed under vacuum leaving a clear yellow oil. The crude 2-(5-ethoxyhept-1-yl)bicyclo[3.3.0]octan-7-one {hexahydro-4-(5-methoxyheptyl)-2(1H)-pentalenone} is chromatographed on silica gel and subsequently kugelrohred under vacuum leaving compound VI as a clear, colorless oil (12 g, 0.045 moles).

後処理

  1. customThe solvent is removed under vacuum
  2. customleaving a clear yellow liquid
  3. additionis slowly added
  4. filtrationthe solution filtered
  5. washThe ether layer is washed with brine (100 ml)
  6. customThe ether layer is separated
  7. dry with materialdried over sodium sulfate
  8. customThe solvent is removed under vacuum
  9. customleaving a clear yellow oil
  10. customis chromatographed on silica gel

出典と根拠

ORDレコード
ord-5586ed485caa4d9b8f9c63a598b19c31
出典データセット
uspto-grants-1989_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04855322

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート