HCID 521386, 화합물 → 1,1-Diphenylethane-1,2-diamine

HRID 441065노트

반응식

HRID 441065 반응식
[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

참가 물질

4

반응물 2

HCID 521386HCID 521386, 화합물HCID 21225700Diisobutylaluminumhydride

생성물 1

HCID 178267441,1-Diphenylethane-1,2-diamine수율 92.8%

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
-20 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-412cdacd613346868d97cc6cecac3881
출처 데이터셋
uspto-grants-1996_05
특허 번호
US05521220

반응 노트

불러오는 중…