Phthaloyl chloride → 2-Fluoromethyl-2-phthalimido-5-methoxypentanenitrile

HRID 1252564ノート

反応式

HRID 1252564 の反応式
[F:1][CH2:2][C:3]([NH2:11])([CH2:6][CH2:7][CH2:8][O:9][CH3:10])[C:4]#[N:5].C(N(CC)CC)C.[C:19](Cl)(=[O:29])[C:20]1[C:21](=[CH:25][CH:26]=[CH:27][CH:28]=1)[C:22](Cl)=[O:23]>C(Cl)Cl>[F:1][CH2:2][C:3]([N:11]1[C:22](=[O:23])[C:21]2=[CH:25][CH:26]=[CH:27][CH:28]=[C:20]2[C:19]1=[O:29])([CH2:6][CH2:7][CH2:8][O:9][CH3:10])[C:4]#[N:5]

参加物

5

反応物 3

HCID 6955Phthaloyl chlorideHCID 8471TriethylamineHCID 199663342-Amino-2-(fluoromethyl)-5-methoxypentanenitrile

生成物 1

HCID 199663292-Fluoromethyl-2-phthalimido-5-methoxypentanenitrile収率 82.7%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a solution of 2-fluoromethyl-2-amino-5-methoxypentanenitrile (1.62 g, 10 mmol) and triethylamine (2.02 g, 20 mmol) in methylene chloride (30 ml), cooled to -20° C., is added phthaloyldichloride (2.03 g, 10 mmol) in methylene chloride (10 ml). The mixture is allowed to warm up to room temperature overnight. After washing with water, 1N HCl, water again, and drying (Na2SO4), the solvent is removed under reduced pressure to give 2.4 g of crude material. This is purified by chromatography on silica (ethyl acetate/petroleum ether 3:7).

後処理

  1. washAfter washing with water, 1N HCl, water again
  2. dry with materialdrying (Na2SO4)
  3. customthe solvent is removed under reduced pressure

出典と根拠

ORDレコード
ord-f102d11c384048eeaac8cb3e971c5ea6
出典データセット
uspto-grants-1988_05
特許番号
US04743691

反応ノート

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