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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Water → HCID 11287409, 화합물

HRID 1791026
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HRID 1791026 반응식
[CH2:1]=[C:2]1[CH2:8][CH:7](S(C2C=CC=CC=2)(=O)=O)[C:6]2[CH:18]=[C:19]([C:22]([O:24][CH3:25])=[O:23])[CH:20]=[CH:21][C:5]=2[O:4][CH2:3]1.P([O-])([O-])(O)=O.[Na+].[Na+].CO.O1CCCC1.O>[Na].[Hg].ClCCl>[CH2:1]=[C:2]1[CH2:8][CH2:7][C:6]2[CH:18]=[C:19]([C:22]([O:24][CH3:25])=[O:23])[CH:20]=[CH:21][C:5]=2[O:4][CH2:3]1
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7

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HCID 962WaterHCID 24203Sodium Phosphate, DibasicHCID 11439769HCID 11439769, 화합물HCID 21899815MeOH tetrahydrofuran

생성물 1

HCID 11287409HCID 11287409, 화합물

시약·촉매·용매 2

HCID 9837419Sodium amalgam촉매
HCID 6344
Dichloromethane
용매

실험 절차

728 mg (0.95 mmol) of 3% sodium amalgam are added portionwise at 0° C. to a suspension of 85 mg (0.23 mmol) of methyl 3-methylene-5-(phenylsulfonyl)-2,3,4,5-tetrahydro-1-benzoxepin-7-carboxylate, prepared according to example 1, and of 116 mg (0.95 mmol) of sodium hydrogenphosphate in 10 ml of a 1/1 methanol/tetrahydrofuran binary mixture. The reaction medium is subsequently stirred at ambient temperature for 4 hours. After addition of water and dichloromethane and filtering off the mercury, the phases are separated and the aqueous phase is extracted 3 times with dichloromethane. The combined organic phases are washed with a slightly acidic aqueous solution and then with brine. After drying and then concentrating under vacuum, 49 mg (98%) of methyl 3-methylene-2,3,4,5-tetrahydro-1-benzoxepin-7-carboxylate are obtained without additional purification in the form of an oil; 1H NMR (300 MHz, CDCl3): 2.53. (m, 2H), 2.93 (m, 2H), 3.89 (s, 3H), 4.49 (s, 2H), 5.0 (d, J=4.1 Hz, 2H), 7.0 (d, J=8.1 Hz, 1H), 7.86 (m, 2H).

후처리

  1. customprepared
  2. filtrationfiltering off the mercury
  3. customthe phases are separated
  4. extractionthe aqueous phase is extracted 3 times with dichloromethane
  5. washThe combined organic phases are washed with a slightly acidic aqueous solution
  6. customAfter drying
  7. concentrationconcentrating under vacuum, 49 mg (98%) of methyl 3-methylene-2,3,4,5-tetrahydro-1-benzoxepin-7-carboxylate
  8. customare obtained without additional purification in the form of an oil

출처 및 근거

ORD 기록
ord-0688c3ac6a054939b48bf4505142ac19
출처 데이터셋
uspto-grants-2006_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07071340B2

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