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

HRID 1252564

반응식

HRID 1252564 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 199663292-Fluoromethyl-2-phthalimido-5-methoxypentanenitrile수율 82.7%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-f102d11c384048eeaac8cb3e971c5ea6
출처 데이터셋
uspto-grants-1988_05
특허 번호
US04743691

연결된 노트

불러오는 중…