Triethylamine → HCID 137328355、化合物

HRID 1092372ノート

反応式

HRID 1092372 の反応式
[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]

参加物

5

反応条件

温度
0 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-09688436a97d4243bc8e302032c81875
出典データセット
uspto-grants-2012_03
特許番号
US08129428B2

反応ノート

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