Hydrochloric Acid → HCID 15062459、化合物

HRID 1938571

反応式

HRID 1938571 の反応式
Br[C:2]1[CH:7]=[C:6]([Br:8])[CH:5]=[CH:4][C:3]=1[O:9][CH3:10].C([Li])CCC.[CH3:16][Si:17](Cl)([CH3:19])[CH3:18].Cl>C(OCC)C>[Br:8][C:6]1[CH:5]=[CH:4][C:3]([O:9][CH3:10])=[CH:2][C:7]=1[Si:17]([CH3:19])([CH3:18])[CH3:16]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 6397ChlorotrimethylsilaneHCID 270112,4-DibromoanisoleHCID 178418339Butyllithium

生成物 1

HCID 15062459HCID 15062459、化合物

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

To a solution of 2,4-dibromoanisole (13.3 g, 50 mmol) in diethyl ether (50 ml) at 0° C. was added over 20 min 1.5M butyllithium (33.4 ml) and the reaction was allowed to react 15 min at 0° C. Then trimethylsilylchloride (5.43 g, 50 mmol) in diethyl ether (20 ml) was added over 10 min and the resulting mixture was stirred 18 hours at room temperature. At 0° C. 3N HCl (50 ml) was added and the organic layer was separated, washed with water, brine, dried over MgSO4 and concentrated. 4-Bromo-3-trimethylsilylanisole was purified by chromatography on silica gel (eluted with cyclohexane) as a colorless oil.

後処理

  1. customto react 15 min at 0° C
  2. customAt 0° C
  3. customthe organic layer was separated
  4. washwashed with water, brine
  5. dry with materialdried over MgSO4
  6. concentrationconcentrated
  7. custom4-Bromo-3-trimethylsilylanisole was purified by chromatography on silica gel (eluted with cyclohexane) as a colorless oil

出典と根拠

ORDレコード
ord-de584600313b432499139c84fb61dd66
出典データセット
uspto-grants-1997_12
特許番号
US05693668

関連ノート

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