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Methyl iodide → HCID 58120020, 화합물

HRID 456213
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HRID 456213 반응식
[CH2:1]([O:3][C:4](=[O:23])[CH2:5][C:6]1[CH:11]=[CH:10][C:9]([O:12][CH3:13])=[C:8]([B:14]2[O:18][C:17]([CH3:20])([CH3:19])[C:16]([CH3:22])([CH3:21])[O:15]2)[CH:7]=1)[CH3:2].IC.[CH3:26][Si](C)(C)N[Si](C)(C)C.[Na]>C1COCC1>[CH2:1]([O:3][C:4](=[O:23])[CH:5]([C:6]1[CH:11]=[CH:10][C:9]([O:12][CH3:13])=[C:8]([B:14]2[O:15][C:16]([CH3:22])([CH3:21])[C:17]([CH3:20])([CH3:19])[O:18]2)[CH:7]=1)[CH3:26])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 45051731Sodium hexamethyidisilazaneHCID 58120060[4-Methoxy-3-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)-phenyl]-acetic acid ethyl ester

생성물 1

HCID 58120020HCID 58120020, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To [4-methoxy-3-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)-phenyl]-acetic acid ethyl ester (0.100 g, 0.31 mmol) and iodomethane (0.04 mL, 0.63 mmol) in THF (5 mL) at −78° C. was added sodium hexamethyldisilazane (1M in THF; 0.63 mL, 0.63 mmol). The reaction was warmed to room temperature and stirred under N2 for 1 hour, and then quenched with H2O and partitioned between EtOAc and H2O. The aqueous layer was separated and extracted with EtOAc, and the combined organic layers were dried over MgSO4, filtered, and concentrated to give the title compound.

후처리

  1. customquenched with H2O
  2. custompartitioned between EtOAc and H2O
  3. customThe aqueous layer was separated
  4. extractionextracted with EtOAc
  5. dry with materialthe combined organic layers were dried over MgSO4
  6. filtrationfiltered
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-e05d10193b844a1fac68dfb408fdc7be
출처 데이터셋
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08497381B2

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