Benzylamine → N-[(Trimethylsilyl)methyl]benzylamine

HRID 557927

反応式

HRID 557927 の反応式
Cl[CH2:2][Si:3]([CH3:6])([CH3:5])[CH3:4].[CH2:7]([NH2:14])[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.[OH-].[Na+]>>[CH2:7]([NH:14][CH2:2][Si:3]([CH3:6])([CH3:5])[CH3:4])[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1

参加物

4

反応物 3

HCID 7504BenzylamineHCID 14798Sodium HydroxideHCID 75361Silane, (chloromethyl)trimethyl-

生成物 1

HCID 353458N-[(Trimethylsilyl)methyl]benzylamine

反応条件

温度
200 °C

実験手順

Into a round bottom 3-neck flask equipped with a nitrogen flow, a magnetic stirrer, and a fried richs condenser was added (chloromethyl)trimethylsilane (0.100 mol). To the flask was added benzylamine (0.300 mol), with stirring, and the resulting solution heated at 200° C. for 2.5 hours. Sodium hydroxide aqueous solution (0.1N) was added in order to hydrolyze the white organic salt that had formed. The mixture was extracted with ether and the ether layer was dried over magnesium sulfate and concentrated under reduced pressure through a Vigreux column to give the product at b.p. 68-72° C./0.7-0.8 mm.

後処理

  1. customInto a round bottom 3-neck flask equipped with a nitrogen flow, a magnetic stirrer, and a fried richs condenser
  2. customhad formed
  3. extractionThe mixture was extracted with ether
  4. dry with materialthe ether layer was dried over magnesium sulfate
  5. concentrationconcentrated under reduced pressure through a Vigreux column
  6. customto give the product at b.p. 68-72° C./0.7-0.8 mm

出典と根拠

ORDレコード
ord-096651746a0848e689f9e72cc3bd31e8
出典データセット
uspto-grants-2011_11
特許番号
US08058288B2

関連ノート

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