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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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1-(5-Bromo-2-methoxyphenyl)adamantane → 6-[3-(1-Adamantyl)-4-methoxyphenyl]-2-bromonaphthalene

HRID 1991922
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HRID 1991922 반응식
[Li]C(C)(C)C.[C:6]12([C:16]3[CH:17]=[C:18](Br)[CH:19]=[CH:20][C:21]=3[O:22][CH3:23])[CH2:15][CH:10]3[CH2:11][CH:12]([CH2:14][CH:8]([CH2:9]3)[CH2:7]1)[CH2:13]2.FC(F)(F)S(O[C:31]1[C:40]2[C:35](=[CH:36][C:37]([Br:41])=[CH:38][CH:39]=2)[CH:34]=[CH:33][CH:32]=1)(=O)=O>C1COCC1.[Cl-].[Cl-].[Zn+2].C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[C:6]12([C:16]3[CH:17]=[C:18]([C:32]4[CH:31]=[C:40]5[C:35](=[CH:34][CH:33]=4)[CH:36]=[C:37]([Br:41])[CH:38]=[CH:39]5)[CH:19]=[CH:20][C:21]=3[O:22][CH3:23])[CH2:7][CH:8]3[CH2:9][CH:10]([CH2:11][CH:12]([CH2:14]3)[CH2:13]1)[CH2:15]2
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참가 물질

7

반응물 3

HCID 32850241-(5-Bromo-2-methoxyphenyl)adamantaneHCID 601611326-Bromonaphthalenyl trifluoromethanesulphonateHCID 178418306HCID 178418306, 화합물

생성물 1

HCID 591298026-[3-(1-Adamantyl)-4-methoxyphenyl]-2-bromonaphthalene수율 34.4%

시약·촉매·용매 3

HCID 3007855Zincchloride촉매
HCID 178418397
HCID 178418397, 화합물
촉매
HCID 8028Tetrahydrofuran용매3회

실험 절차

t-BuLi (159 μl, 1.4 M, 0.22 mmol) was added, dropwise, onto a mixture of 3-(1-adamantyl)-1-bromo-4-methoxybenzene (50 mg, 0.16 mmol) and anh. THF (1 ml) under atmosphere of Ar and at −78° C., and the mixture was kept in stirring for 1 hour. After this time, the reaction was allowed to evolve at room temperature, a solution of ZnCl2 (21 mg, 0.16 mmol) in anhydrous THF (0.4 mL) was added and was stirred for 1 more hour. Next, a solution of 6-bromonaphthalenyl trifluoromethanesulphonate (40 mg, 0.13 mmol), Pd(PPh3)4 (9 mg, 0.008 mmol) and anh. THF (0.2 ml) was added and the reaction was kept at room temperature for 16 h. Finally, the reaction was neutralized with HCl (1 M) and extractions with Et2O (3×2 ml) were carried out. The organic phase was washed with sat NaCl (3×3 ml) and H2O (3×3 ml), was dried with MgSO4 and was evaporated to dryness. A crude (58 mg) in form of a yellow solid was obtained, which was recrystallized with the minimum volume of toluene at reflux (0.2 ml), giving the title compound (20 mg, 29%) as a pale yellow powder. The spectroscopic data coincide with those of the Example 4.

후처리

  1. customat −78° C.
  2. customto evolve at room temperature
  3. stirringwas stirred for 1 more hour
  4. waitthe reaction was kept at room temperature for 16 h
  5. extractionFinally, the reaction was neutralized with HCl (1 M) and extractions with Et2O (3×2 ml)
  6. washThe organic phase was washed with sat NaCl (3×3 ml) and H2O (3×3 ml)
  7. dry with materialwas dried with MgSO4
  8. customwas evaporated to dryness
  9. customA crude (58 mg) in form of a yellow solid was obtained
  10. customwhich was recrystallized with the minimum volume of toluene
  11. temperatureat reflux (0.2 ml)

출처 및 근거

ORD 기록
ord-bcf522dc462f4b4b8fb30a3379c03ca6
출처 데이터셋
uspto-grants-2010_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07645910B2

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