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[(Diphenylmethylene)amino]acetonitrile → 2-(Benzhydrylideneamino)-3-quinolin-4-yl-propionitrile

HRID 1597360
ノート
印刷プレビュー

反応式

HRID 1597360 の反応式
[CH:1]1[CH:6]=[CH:5][C:4]([C:7]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)=[N:8][CH2:9][C:10]#[N:11])=[CH:3][CH:2]=1.[Li+].CC([N-]C(C)C)C.Cl[CH2:27][C:28]1[C:37]2[C:32](=[CH:33][CH:34]=[CH:35][CH:36]=2)[N:31]=[CH:30][CH:29]=1>C1COCC1>[C:7](=[N:8][CH:9]([CH2:27][C:28]1[C:37]2[C:32](=[CH:33][CH:34]=[CH:35][CH:36]=2)[N:31]=[CH:30][CH:29]=1)[C:10]#[N:11])([C:4]1[CH:3]=[CH:2][CH:1]=[CH:6][CH:5]=1)[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 612957[(Diphenylmethylene)amino]acetonitrileHCID 2724682Lithium diisopropylamideHCID 123557014-(Chloromethyl)quinoline

生成物 1

HCID 234992122-(Benzhydrylideneamino)-3-quinolin-4-yl-propionitrile収率 26.3%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
-78 °C

実験手順

To N-(Diphenylmethylene)aminoacetonitrile (0.360 g, 1.633 mmol) in 10 ml of anhydrous THF and HMPA (hexamethyl phosphoramidite) (0.38 ml, 2.12 mmol), at −78° C., LDA (2.0 M, 1.06 ml, 2.12 mmol) was added dropwise over a period of 5 minutes. The color of solution turns from colorless to yellow to dark brown. It was then stirred at −78° C. for one hour. 4-Chloromethylquinoline (0.29 g, 1.63 mmol) was added dropwise over a period of 5 minutes and the reaction mixture was slowly brought to room temperature over a period of five minutes. The reaction mixture was quenched by addition of ice and partitioned between EtOAc (20 ml) and water (5 ml). The organic layer was dried over sodium sulfate, filtered concentrated and column purified (hexanes:EtOAc; 3.5:1.5) to give 0.155 g (26%) of the product as a syrup, which was used as such for the subsequent step.

後処理

  1. waitthe reaction mixture was slowly brought to room temperature over a period of five minutes
  2. customThe reaction mixture was quenched by addition of ice
  3. custompartitioned between EtOAc (20 ml) and water (5 ml)
  4. dry with materialThe organic layer was dried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customcolumn purified (hexanes:EtOAc; 3.5:1.5)

出典と根拠

ORDレコード
ord-cf3a69b1f80e4f7ea1ad55e5ec84ae6a
出典データセット
uspto-grants-2001_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06294566B1

反応ノート

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