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

HCID 15735544、化合物 → HCID 15735587、化合物

HRID 704605
ノート
印刷プレビュー

反応式

HRID 704605 の反応式
[CH:1]1(/[CH:7]=[C:8](/[CH2:14][P:15]([O:21]CC)([CH2:17][CH:18]([CH3:20])[CH3:19])=[O:16])\[C:9]([O:11]CC)=[O:10])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.C1(/C=C(\CP(O)(CC(C)C)=O)/C(OCC)=O)CCCCC1.C1(/C=C(/CP(O)(CC(C)C)=O)\C(OCC)=O)CCCCC1.OP(C/C(=C\C(C)CCC(O)=O)/C(O)=O)(CC(C)C)=O>Cl.C(OCCCC)(=O)C.C(O)C.[OH-].[Na+]>[CH:1]1(/[CH:7]=[C:8](\[CH2:14][P:15]([OH:21])([CH2:17][CH:18]([CH3:19])[CH3:20])=[O:16])/[C:9]([OH:11])=[O:10])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 15735544HCID 15735544、化合物HCID 15735657HCID 15735657、化合物HCID 18643487HCID 18643487、化合物HCID 86744540HCID 86744540、化合物

生成物 1

HCID 15735587HCID 15735587、化合物収率 49.5%

試薬・触媒・溶媒 3

HCID 702Ethanol溶媒
HCID 14798Sodium Hydroxide溶媒
HCID 20072624HCID 20072624、化合物溶媒

実験手順

A solution of 11.1 g (32.2 millimoles) of ethyl (E)-3-cyclohexyl-2-(ethoxyisobutylphosphinoyl)methylpropenoate in 100 ml of 4.3 N hydrogen chloride-butyl acetate was heated in a sealed tube for 48 hours. After cooling, the solvent was evaporated under reduced pressure to give a mixture of ethyl (Z)-3-cyclohexyl-2-(hydroxyisobutylphosphinoyl)methylpropenoate and ethyl (E)-3-cyclohexyl-2-(hydroxyisobutylphosphinoyl)methylpropenoate as a pale yellow oil. The (Z):(E) ratio determined by 1H-NMR was 90:10. The mixture was dissolved in a mixture of 32 ml of ethanol and 16 ml of 6 N sodium hydroxide, and heated under reflux for 3 hours. After cooling, the solvent was evaporated under reduced pressure. The residue was dissolved in 100 ml of water and made strongly acidic with hydrochloric acid, whereupon crystals precipitated. The crystals were collected by filtration and recrystallized from methanol-water (2:1) to give 4.6 g (yield 49%) of (Z)-3-cyclohexyl-2-(hydroxyisobutylphosphinoyl)methylpropenoic acid. Its melting point and IR and 1H-NMR were identical with those of the product obtained in Example 5 (b).

後処理

  1. temperatureAfter cooling
  2. customthe solvent was evaporated under reduced pressure
  3. customto give
  4. temperatureheated
  5. temperatureunder reflux for 3 hours
  6. temperatureAfter cooling
  7. customthe solvent was evaporated under reduced pressure
  8. dissolutionThe residue was dissolved in 100 ml of water
  9. customprecipitated
  10. filtrationThe crystals were collected by filtration
  11. customrecrystallized from methanol-water (2:1)

出典と根拠

ORDレコード
ord-581971c643fe4c2091847840fec91167
出典データセット
uspto-grants-1991_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04988681

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