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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Ethanol → HCID 11138604, 화합물

HRID 2082583
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HRID 2082583 반응식
C(O)C.[Cl:4][C:5]1[C:10]([CH3:11])=[C:9](Br)[CH:8]=[C:7]([S:13]([CH3:16])(=[O:15])=[O:14])[C:6]=1[CH3:17].C([O-])(=O)C.[Na+].[H][H]>[Pd].O>[Cl:4][C:5]1[C:6]([CH3:17])=[C:7]([S:13]([CH3:16])(=[O:15])=[O:14])[CH:8]=[CH:9][C:10]=1[CH3:11]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 702EthanolHCID 517045Sodium AcetateHCID 10859468HCID 10859468, 화합물HCID 178418361HCID 178418361, 화합물

생성물 1

HCID 11138604HCID 11138604, 화합물

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 962
Water
용매

실험 절차

30 ml of ethanol was added to 1.0 g of the crude 2-chloro-4-bromo-6-methylsulfonyl-m-xylene obtained in Example 2, and 0.1 g of 5% palladium active carbon and 1.0 g of anhydrous sodium acetate were further added thereto. The reactor was sealed, and was substituted with hydrogen, then stirring at room temperature for 7 hours. 30 ml of water was added to the reaction liquor, and was concentrated under reduced pressure. 30 ml of EDC was further added thereto, and the resultant mixture was filtered. The EDC layer was taken out from the filtrate, and was washed with 20 ml of water and then with 10 ml of a saturated aqueous solution of common salt, and was dried over anhydrous sodium sulfate. The EDC layer thus obtained was concentrated under reduced pressure and was dried to a solid to obtain 0.7 g of a crude product of the above-identified aimed compound (purity measured by gas chromatography: 75.6%). The crude product thus obtained was recrystallized by methanol to obtain the above-identified aimed compound.

후처리

  1. additionwere further added
  2. customThe reactor was sealed
  3. concentrationwas concentrated under reduced pressure
  4. addition30 ml of EDC was further added
  5. filtrationthe resultant mixture was filtered
  6. washwas washed with 20 ml of water
  7. dry with materialwith 10 ml of a saturated aqueous solution of common salt, and was dried over anhydrous sodium sulfate
  8. customThe EDC layer thus obtained
  9. concentrationwas concentrated under reduced pressure
  10. customwas dried to a solid
  11. customto obtain 0.7 g of a crude product of the above-identified aimed compound (purity measured by gas chromatography: 75.6%)
  12. customThe crude product thus obtained
  13. customwas recrystallized by methanol

출처 및 근거

ORD 기록
ord-b1628a3f465f45abbe9a41ee5dc16d1f
출처 데이터셋
uspto-grants-1993_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05189224

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