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Boron tribromide → HCID 21957107, 화합물

HRID 1357675
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HRID 1357675 반응식
[ClH:1].[N:2]1([CH2:8][CH2:9][O:10][C:11]2[CH:37]=[CH:36][C:14]([O:15][C:16]3[C:25]4[C:20](=[CH:21][C:22]([O:26]C)=[CH:23][CH:24]=4)[CH:19]=[CH:18][C:17]=3[C:28]3[CH:33]=[CH:32][CH:31]=[C:30]([O:34]C)[CH:29]=3)=[CH:13][CH:12]=2)[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3]1.B(Br)(Br)Br>C(Cl)Cl>[ClH:1].[N:2]1([CH2:8][CH2:9][O:10][C:11]2[CH:12]=[CH:13][C:14]([O:15][C:16]3[C:25]4[C:20](=[CH:21][C:22]([OH:26])=[CH:23][CH:24]=4)[CH:19]=[CH:18][C:17]=3[C:28]3[CH:33]=[CH:32][CH:31]=[C:30]([OH:34])[CH:29]=3)=[CH:36][CH:37]=2)[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 25134Boron tribromideHCID 98713381-[4-[2-(1-Piperidinyl)-ethoxy]phenoxy]-2-(3-methoxyphenyl)-6-methoxynaphthalene hydrochloride

생성물 1

HCID 21957107HCID 21957107, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
0 °C

실험 절차

A solution was prepared of 1.5 g (2.9 mmol) of 1-[4-[2-(1-piperidinyl)ethoxy]phenoxy]-2-(3-methoxyphenyl)-6-methoxynaphthalene hydrochloride in 30 mL of CH2Cl2 and the solution was cooled to 0° C. under a nitrogen atmosphere. To this solution was added 1.09 mL (2.89g, 11.5 mmol) of BBr3 and the reaction was allowed to proceed for two hours at 0° C. The reaction was quenched by the addition of aqueous NaHCO3 solution (50 mL). The reaction mixture was extracted with CHCl3. The organic layer was washed with brine, dried with Na2SO4, and evaporated to dryness. The residue was suspended in THF and filtered. To the filtrate was added 1 mL of 5N HCl and the solvents were removed by evaporation. This yielded 0.99 g of the title compound as a tan amorphous powder.

후처리

  1. customThe reaction was quenched by the addition of aqueous NaHCO3 solution (50 mL)
  2. extractionThe reaction mixture was extracted with CHCl3
  3. washThe organic layer was washed with brine
  4. dry with materialdried with Na2SO4
  5. customevaporated to dryness
  6. filtrationfiltered
  7. additionTo the filtrate was added 1 mL of 5N HCl
  8. customthe solvents were removed by evaporation

출처 및 근거

ORD 기록
ord-d9ab73de98584e22aae0e127483d0392
출처 데이터셋
uspto-grants-2003_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06593345B1

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