Triethylamine → HCID 137328355, 화합물

HRID 1917004노트

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HRID 1917004 반응식
[Br:1][C:2]1[CH:3]=[C:4]([OH:8])[CH:5]=[CH:6][CH:7]=1.CCN(CC)CC.[CH3:16][Si:17](Cl)([CH3:20])[CH2:18][CH3:19]>C1COCC1>[Br:1][C:2]1[CH:3]=[C:4]([CH:5]=[CH:6][CH:7]=1)[O:8][CH2:19][CH2:18][SiH:17]([CH3:20])[CH3:16]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 115633-BromophenolHCID 138863Ethyldimethylchlorosilane

생성물 1

HCID 137328355HCID 137328355, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
0 °C

실험 절차

To a stirred solution of 3-bromophenol (0.60 g, 3.47 mmol) in dry THF (15 mL) under nitrogen was added Et3N (0.48 mL, 3.47 mmol). A clear yellow solution formed immediately; after cooling to 0° C., dimethylethylsilyl chloride (0.43 g, 0.49 mL, 3.47 mmol) was added by syringe over a period of 10 minutes. The yellow color disappeared in 10 min, and a white cloudy solution formed. After 3 hr the thick reaction mixture was filtered, washed with 15 mL of hexane, and filtered again. Concentration gave a clear oil (quantitative weight recovery) that was used in the next step without any purification.

후처리

  1. customA clear yellow solution formed immediately
  2. customa white cloudy solution formed
  3. filtrationAfter 3 hr the thick reaction mixture was filtered
  4. washwashed with 15 mL of hexane
  5. filtrationfiltered again
  6. concentrationConcentration
  7. customgave a clear oil (quantitative weight recovery) that
  8. customwas used in the next step without any purification

출처 및 근거

ORD 기록
ord-60601e8ef4dc439b981fcc7cb2d00de1
출처 데이터셋
uspto-grants-2013_12
특허 번호
US08618162B2

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