Sodium Sulfate → 2-Amino-3-phenoxypropanenitrile

HRID 1029809

反応式

HRID 1029809 の反応式
[O:1]([CH2:8][C:9]#[N:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[H-].C([Al+]CC(C)C)C(C)C.[C-:21]#[N:22].C([Al+]CC)C.S([O-])([O-])(=O)=O.[Na+].[Na+]>C1(C)C=CC=CC=1.CO>[NH2:10][CH:9]([CH2:8][O:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1)[C:21]#[N:22]

参加物

7

反応物 4

HCID 24436Sodium SulfateHCID 241641PhenoxyacetonitrileHCID 16686413Diethyl aluminum cyanideHCID 21225700Diisobutylaluminumhydride

生成物 1

HCID 139832712-Amino-3-phenoxypropanenitrile収率 22%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 1140Toluene溶媒

反応条件

温度
0 °C

実験手順

5 millimoles (0.665 g) of phenoxy-acetonitrile are dissolved in 8 ml of anhydrous toluene at 0° C., under an argon atmosphere 7.5 millimoles of a toluenic solution 1.5M of diisobutylaluminum hydride (5 ml) are added dropwise, at this temperature. The stirring is maintained for 1 hour at 0° C., then 5.9 ml (1.3 eq) of diethylaluminum cyanide are added. The reaction mixture is stirred for 3 hours at room temperature, then hydrolyzed with 4 ml of methanol and pasty sodium sulfate. After purification by high pressure liquid chromatography on silica, there are obtained 0.182 g of 2-amino-3-phenoxy-propionitrile, in form of a cream-colored solid- state product; M.P. 65° C., yield: 22%.

後処理

  1. additionare added dropwise, at this temperature
  2. customAfter purification by high pressure liquid chromatography on silica, there

出典と根拠

ORDレコード
ord-2ff9a1cf07cb4a51a21831f8a6fc177a
出典データセット
uspto-grants-1992_04
特許番号
US05103019

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