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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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6-{2-[2,4-dichloro-6-(2-methoxyethoxymethoxy) phenyl]ethyl}-3,4,5,6-tetrahydro-4-hydroxy-2H-pyran-2-one → 6-{2-(2,4-Dichloro-6-hydroxyphenyl)-ethyl}-3,4,5,6-tetrahydro-4-hydroxy-2H-pyran-2-one

HRID 986059
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HRID 986059 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[C:4]([O:9]COCCOC)[C:3]=1[CH2:16][CH2:17][CH:18]1[O:23][C:22](=[O:24])[CH2:21][CH:20]([OH:25])[CH2:19]1>C(Cl)Cl.[Br-].[Zn+2].[Br-]>[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[C:4]([OH:9])[C:3]=1[CH2:16][CH2:17][CH:18]1[O:23][C:22](=[O:24])[CH2:21][CH:20]([OH:25])[CH2:19]1
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4

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HCID 135531946-{2-[2,4-dichloro-6-(2-methoxyethoxymethoxy) phenyl]ethyl}-3,4,5,6-tetrahydro-4-hydroxy-2H-pyran-2-one

생성물 1

HCID 135531966-{2-(2,4-Dichloro-6-hydroxyphenyl)-ethyl}-3,4,5,6-tetrahydro-4-hydroxy-2H-pyran-2-one수율 16.4%

시약·촉매·용매 2

HCID 10421208Zinc bromide촉매HCID 6344Dichloromethane용매

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온도
20 °C

실험 절차

Zinc bromide (2.4 g, 10 mmole) was added to a solution of 6-{2-[2,4-dichloro-6-(2-methoxyethoxymethoxy) phenyl]ethyl}-3,4,5,6-tetrahydro-4-hydroxy-2H-pyran-2-one (780 mg, 2 mmole) in methylene chloride (12 ml). The resulting mixture was stirred at 20° C. for 2 hours, then quenched with saturated sodium bicarbonate solution (50 ml) and diluted with ether (200 ml). The ethereal layer was washed with brine, dried over MgSO4, filtered and evaporated. The residue was chromatographed on a 50 mm low-pressure column with 6 inches of silica gel (230-400 mesh). The column was eluted with 470 ml of methylene chloride-acetone (4:1, v:v). The next 330 ml provided the title compound as a golden glass (100 mg., 16%): pmr (CDCl3)δ2.62 (2H, d), 4.29 (H, m), 4.78 (H, m), 6.87 (2H, s).

후처리

  1. customquenched with saturated sodium bicarbonate solution (50 ml)
  2. additiondiluted with ether (200 ml)
  3. washThe ethereal layer was washed with brine
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. customevaporated
  7. customThe residue was chromatographed on a 50 mm low-pressure column with 6 inches of silica gel (230-400 mesh)
  8. washThe column was eluted with 470 ml of methylene chloride-acetone (4:1, v:v)

출처 및 근거

ORD 기록
ord-8194bd8a3b384bcbb930c36bb46a90e5
출처 데이터셋
uspto-grants-1987_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04710513

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