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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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M-Phenylenediamine → HCID 22674043, 화합물

HRID 1005671
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HRID 1005671 반응식
[C:1]1([NH2:8])[CH:6]=[CH:5][CH:4]=[C:3]([NH2:7])[CH:2]=1.[CH3:9][CH2:10][O:11][C:12]([CH2:14][C:15]([C:17](OCC)=O)=O)=[O:13].P(Cl)(Cl)([Cl:24])=O.[OH-].[Na+]>C(Cl)(Cl)Cl>[NH2:7][C:3]1[CH:2]=[C:1]2[C:6]([C:14]([C:12]([O:11][CH2:10][CH3:9])=[O:13])=[CH:15][C:17]([Cl:24])=[N:8]2)=[CH:5][CH:4]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 7935M-PhenylenediamineHCID 14798Sodium HydroxideHCID 24813Phosphorus oxychlorideHCID 66951Diethyl oxalacetate

생성물 1

HCID 22674043HCID 22674043, 화합물

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

To 25 g (231 mmol) of m-phenylenediamine was added 43 g (231 mmol) of diethyl oxaloacetate, followed by stirring at 160 degrees for 1 hour. After standing to cool, the crystals were washed with methanol. To a solution of the crystals (3.0 g, 13 mmol) in chloroform (30 ml) was added phosphorus oxychloride (3.6 ml), followed by heating under reflux for 1 hour. After standing to cool, the reaction mixture was poured onto ice water, basified with 1 N sodium hydroxide aqueous solution, and the resulting crystals were collected by filtration. The crystals were washed with tetrahydrofuran and the filtrate was evaporated, to give 4.85 g of the title compound.

후처리

  1. temperatureto cool
  2. washthe crystals were washed with methanol
  3. temperatureby heating
  4. temperatureunder reflux for 1 hour
  5. temperatureto cool
  6. additionthe reaction mixture was poured onto ice water
  7. filtrationthe resulting crystals were collected by filtration
  8. washThe crystals were washed with tetrahydrofuran
  9. customthe filtrate was evaporated

출처 및 근거

ORD 기록
ord-a9cf8abb335e4d9eaf67514f6fff8903
출처 데이터셋
uspto-grants-2004_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06787534B2

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