Chloride → N-[(Ethoxydimethylsilyl)methyl]cyclohexanamine

HRID 2220554ノート

反応式

HRID 2220554 の反応式
[CH:1]1([NH2:7])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.Cl[CH2:9][Si:10]([O:13][CH2:14][CH3:15])([CH3:12])[CH3:11].[Cl-]>>[CH:1]1([NH:7][CH2:9][Si:10]([O:13][CH2:14][CH3:15])([CH3:12])[CH3:11])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1

参加物

4

反応物 3

HCID 312ChlorideHCID 7965CyclohexylamineHCID 26073(Chloromethyl)ethoxydimethylsilane

生成物 1

HCID 15965763N-[(Ethoxydimethylsilyl)methyl]cyclohexanamine収率 61%

反応条件

温度
30 °C

実験手順

In a 500 ml three-necked flask having a reflux condenser, KPG stirrer and thermometer, 176 g of commercial cyclohexylamine (water content ≦2%) were heated to 100° C., and 122 g of (chloromethyl)ethoxydimethylsilane were added over the course of 30 min with stirring. After the end of the addition, the mixture was stirred for two hours under reflux and cooled to 30° C., and the white precipitate formed was filtered using a pressure filter, and rinsed with cyclohexylamine. Filtrate and wash solutions were combined and were freed from excess cyclohexylamine under reduced pressure. The subsequent fractional distillation gave 105 g (yield 61%) of (N-cyclohexylaminomethyl)ethoxydimethylsilane having a chloride content of 600 ppm.

後処理

  1. customIn a 500 ml three-necked flask having
  2. additionAfter the end of the addition
  3. stirringthe mixture was stirred for two hours
  4. temperatureunder reflux
  5. customthe white precipitate formed
  6. filtrationwas filtered
  7. filtrationfilter
  8. washrinsed with cyclohexylamine
  9. washFiltrate and wash solutions
  10. distillationThe subsequent fractional distillation

出典と根拠

ORDレコード
ord-ea0d39c98e564b0795e6f12dbc434a17
出典データセット
uspto-grants-2008_08
特許番号
US07417160B2

反応ノート

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