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Trimethylsilyl iodide → HCID 19700501, 화합물

HRID 861886
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인쇄 미리보기

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HRID 861886 반응식
I[Si](C)(C)C.[CH:6]1([C:12]2[CH:21]=[C:20]3[C:15]([CH2:16][CH2:17][C:18]([C:22]([NH:24][C:25]4[CH:30]=[CH:29][C:28]([CH2:31][P:32]([O:37]CC)([O:34]CC)=[O:33])=[CH:27][CH:26]=4)=[O:23])=[CH:19]3)=[CH:14][CH:13]=2)[CH2:11][CH2:10][CH2:9][CH2:8][CH2:7]1>C(Cl)(Cl)(Cl)Cl>[CH:6]1([C:12]2[CH:21]=[C:20]3[C:15]([CH2:16][CH2:17][C:18]([C:22]([NH:24][C:25]4[CH:30]=[CH:29][C:28]([CH2:31][P:32]([OH:37])([OH:34])=[O:33])=[CH:27][CH:26]=4)=[O:23])=[CH:19]3)=[CH:14][CH:13]=2)[CH2:7][CH2:8][CH2:9][CH2:10][CH2:11]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 85247Trimethylsilyl iodideHCID 9805227HCID 9805227, 화합물

생성물 1

HCID 19700501HCID 19700501, 화합물수율 63.4%

시약·촉매·용매 1

HCID 5943Carbon Tetrachloride용매

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온도
0 °C

실험 절차

Iodotrimethylsilane [(CH3)3SiI] (0.458 g) was added to a suspension of 7-cyclohexyl-N-(4-diethoxyphosphorylmethylphenyl)-3,4-dihydronaphthalene-2-carboxamide (0.5 g) in carbon tetrachloride (10 ml) at 0° C. After stirring at 0° C. for 1 hour and then at room temperature for 15 hours, this mixture was concentrated under reduced pressure. To the residue, methanol (6 ml) was added; this mixture was acidified with 1N HCl and stirred at room temperature for 30 minutes. The resulting crystals were collected by filtration and recrystallized from methanol-water to yield 7-cyclohexyl-N-(4-phosphonomethylphenyl)-3,4-dihydronaphthalene-2-carboxamide (0.28 g, 63%) as pale yellow prisms having a melting point of 203°-205° C.

후처리

  1. waitat room temperature for 15 hours
  2. concentrationthis mixture was concentrated under reduced pressure
  3. additionTo the residue, methanol (6 ml) was added
  4. stirringstirred at room temperature for 30 minutes
  5. filtrationThe resulting crystals were collected by filtration
  6. customrecrystallized from methanol-water

출처 및 근거

ORD 기록
ord-48e32cd2f2ae414ea263df18048a0a3b
출처 데이터셋
uspto-grants-1998_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05716944

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