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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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HCID 15735544, 화합물 → HCID 15735587, 화합물

HRID 704605
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HRID 704605 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 15735544HCID 15735544, 화합물HCID 15735657HCID 15735657, 화합물HCID 18643487HCID 18643487, 화합물HCID 86744540HCID 86744540, 화합물

생성물 1

HCID 15735587HCID 15735587, 화합물수율 49.5%

시약·촉매·용매 3

HCID 702Ethanol
용매
HCID 14798Sodium Hydroxide용매
HCID 20072624HCID 20072624, 화합물용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-581971c643fe4c2091847840fec91167
출처 데이터셋
uspto-grants-1991_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04988681

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