Chloroacetyl chloride → N-chloromethylcarbonyl-2-azatricyclo-[4.3.1.14,8]undecane

HRID 963468ノート

反応式

HRID 963468 の反応式
[CH:1]12[CH2:11][CH:6]3[CH2:7][CH:8]([CH2:10][CH:4]([CH2:5]3)[CH2:3][NH:2]1)[CH2:9]2.[Cl:12][CH2:13][C:14](Cl)=[O:15]>ClCCl.O>[Cl:12][CH2:13][C:14]([N:2]1[CH2:3][CH:4]2[CH2:10][CH:8]3[CH2:7][CH:6]([CH2:11][CH:1]1[CH2:9]3)[CH2:5]2)=[O:15]

参加物

5

反応物 2

HCID 6577Chloroacetyl chlorideHCID 322724-Azatricyclo[4.3.1.13,8]undecane

生成物 1

HCID 86752745N-chloromethylcarbonyl-2-azatricyclo-[4.3.1.14,8]undecane収率 73.1%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒2 回

実験手順

To a solution of 2-azatricyclo[4.3.1.14,8 ]undecane (0.30 g) in dichloromethane (4 ml) and water (0.4 ml) was added dropwise a solution of chloroacetyl chloride (0.26 g) in dichloromethane (2 ml) under stirring at cooling in an ice-bath. The mixture was stirred 2 hours under the same condition and then at ambient temperature overnight. The reaction mixture was washed with IN hydrochloric acid aqueous solution and saturated sodium bicarbonate aqueous solution, and dried over sodium sulfate. Removal of the solvent gave N-chloromethylcarbonyl-2-azatricyclo-[4.3.1.14,8 ]undecane (0.33 g), which was used in a following reaction step without further purification.

後処理

  1. temperatureat cooling in an ice-bath
  2. stirringThe mixture was stirred 2 hours under the same condition
  3. customat ambient temperature
  4. customovernight
  5. washThe reaction mixture was washed with IN hydrochloric acid aqueous solution and saturated sodium bicarbonate aqueous solution
  6. dry with materialdried over sodium sulfate
  7. customRemoval of the solvent

出典と根拠

ORDレコード
ord-a7e93a5b3fce459cbea1916f2deb3d7a
出典データセット
uspto-grants-1998_06
特許番号
US05763437

反応ノート

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