Chloroacetonitrile → HCID 10611289、化合物

HRID 369765

反応式

HRID 369765 の反応式
[O:1]1[C:6]2[CH:7]=[CH:8][CH:9]=[C:10]([N:11]3[CH2:16][CH2:15][NH:14][CH2:13][CH2:12]3)[C:5]=2[O:4][CH2:3][CH2:2]1.[CH2:17]([N:19](CC)CC)[CH3:18].ClCC#N>CN1CCCC1=O>[O:1]1[C:6]2[CH:7]=[CH:8][CH:9]=[C:10]([N:11]3[CH2:16][CH2:15][N:14]([CH2:18][C:17]#[N:19])[CH2:13][CH2:12]3)[C:5]=2[O:4][CH2:3][CH2:2]1

参加物

5

反応物 3

HCID 7856ChloroacetonitrileHCID 8471TriethylamineHCID 65853Eltoprazine

生成物 1

HCID 10611289HCID 10611289、化合物

試薬・触媒・溶媒 1

HCID 13387N-methyl-2-pyrrolidone溶媒

反応条件

温度
100 °C

実験手順

A solution of 1-(1,4-benzodioxan-5-yl)piperazin (11 g) and triethylamine (7 ml) in N-methyl-2-pyrrolidinone was treated dropwise with chloroacetonitrile (4.5 g). After stirring for 2 h at 100° C. the mixture was poured onto ice and extracted with ethyl acetate. The organic phase was washed with water, dried over magnesium sulfate, filtered, and concentrated in vacuo. The product, 1-(1,4-benzodioxan-5-yl)-4-cyanomethylpiperazine, was obtained as an oil (17.4 g) which was sufficiently pure for use in the next step.

後処理

  1. additionwas poured onto ice
  2. extractionextracted with ethyl acetate
  3. washThe organic phase was washed with water
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-af384c9025af431e988eb164518e50de
出典データセット
uspto-grants-2000_10
特許番号
US06140331

関連ノート

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