Methyl iodide → HCID 23023145、化合物

HRID 1477394ノート

反応式

HRID 1477394 の反応式
[Br:1][C:2]1[CH:9]=[CH:8][C:5]([C:6]#[N:7])=[C:4]([CH3:10])[CH:3]=1.[Li+].[CH3:12]C([N-]C(C)C)C.CI>C1COCC1>[Br:1][C:2]1[CH:9]=[CH:8][C:5]([C:6]#[N:7])=[C:4]([CH2:10][CH3:12])[CH:3]=1

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 1442674-Bromo-2-methylbenzonitrileHCID 2724682Lithium diisopropylamide

生成物 1

HCID 23023145HCID 23023145、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of 4-bromo-2-methylbenzonitrile (0.4 g, 2.0 mmol) in dry THF (10 mL) was slowly added LDA (1.3 mL, 1.8 M in THF) at 78° C. and stirred at this temperature for additional 30 min. Methyl iodide (0.15 mL, 2.4 mmol) was added) at 78° C. to the above dark purple solution and the mixture was warmed to room temperature over 3 h. The reaction was quenched with water, extracted with ether, which was then was washed with brine, dried and concentrated. 4-Bromo-2-ethylbenzonitrile (0.34 g) was purified by Combiflash.

後処理

  1. customat 78° C.
  2. customThe reaction was quenched with water
  3. extractionextracted with ether, which
  4. washwas then was washed with brine
  5. customdried
  6. concentrationconcentrated
  7. custom4-Bromo-2-ethylbenzonitrile (0.34 g) was purified by Combiflash

出典と根拠

ORDレコード
ord-3bbdb0ef7502494bbd3f975ca6a9a75b
出典データセット
uspto-grants-2016_08
特許番号
US09403775B2

反応ノート

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