HCID 521386、化合物 → 1,1-Diphenylethane-1,2-diamine

HRID 441065ノート

反応式

HRID 441065 の反応式
[C:1]1([C:7]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)([NH2:10])[C:8]#[N:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[H-].C([Al+]CC(C)C)C(C)C>C1(C)C=CC=CC=1>[C:1]1([C:7]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)([NH2:10])[CH2:8][NH2:9])[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

参加物

4

反応物 2

HCID 521386HCID 521386、化合物HCID 21225700Diisobutylaluminumhydride

生成物 1

HCID 178267441,1-Diphenylethane-1,2-diamine収率 92.8%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
-20 °C

実験手順

α,α-Diphenyl-α-aminoacetonitrile (1.0 gm, 0.0048 mol) was dissolved in 6 ml of toluene and was cooled to -20° C. The solution was treated with 19.2 ml (0.0192 mol) of 1 M diisobutylaluminum hydride (DiBal-H) and stirred at -20° C. for 3 hours. The reaction mixture was quenched with 2.0 ml of methanol followed by 50 ml of water. The reaction mixture was acidified to pH 1.0 and the aqueous phase was extracted with ether several times. The remaining aqueous phase was basified to pH 13 with 2N sodium hydroxide solution and extracted with methylene chloride. The organic phase was dried and evaporated to afford 0.946 g (92%) of the desired material as an oil.

後処理

  1. customThe reaction mixture was quenched with 2.0 ml of methanol
  2. extractionthe aqueous phase was extracted with ether several times
  3. extractionextracted with methylene chloride
  4. customThe organic phase was dried
  5. customevaporated

出典と根拠

ORDレコード
ord-412cdacd613346868d97cc6cecac3881
出典データセット
uspto-grants-1996_05
特許番号
US05521220

反応ノート

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