Water → 2-(5-Fluoropentyl)-2-(3,3,3-trifluoropropyl)malononitrile

HRID 1443558노트

반응식

HRID 1443558 반응식
C(N(S(F)(F)[F:7])CC)C.O[CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][C:16]([CH2:21][CH2:22][C:23]([F:26])([F:25])[F:24])([C:19]#[N:20])[C:17]#[N:18].O>C(Cl)(Cl)Cl>[F:7][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][C:16]([CH2:21][CH2:22][C:23]([F:26])([F:25])[F:24])([C:19]#[N:20])[C:17]#[N:18]

참가 물질

5

반응물 3

HCID 962WaterHCID 123472(Diethylamino)sulfur trifluorideHCID 588790372-(5-Hydroxypentyl)-2-(3,3,3-trifluoropropyl)malononitrile

생성물 1

HCID 866125442-(5-Fluoropentyl)-2-(3,3,3-trifluoropropyl)malononitrile수율 29.8%

시약·촉매·용매 1

HCID 6212Chloroform용매2회

실험 절차

0.29 g of diethylaminosulfur trifluoride was dissolved in 5 ml of chloroform and thereto was added dropwise at 0° C. 0.40 g of 2-(5-hydroxypentyl)-2-(3,3,3-trifluoropropyl)malononitrile dissolved in 3 ml of chloroform. The mixture was stirred at room temperature for 9 hours. Thereafter, water was added to the reaction mixture, followed by extraction with methyl tert-butyl ether. The organic layer was washed successively with water, aqueous saturated sodium hydrogen carbonate and aqueous saturated sodium chloride, dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to obtain 0.12 g of 2-(5-fluoropentyl)-2-(3,3,3-trifluoropropyl)malononitrile (hereinafter, referred to as the present compound (55)).

후처리

  1. additionwas added dropwise at 0° C
  2. extractionfollowed by extraction with methyl tert-butyl ether
  3. washThe organic layer was washed successively with water, aqueous saturated sodium hydrogen carbonate and aqueous saturated sodium chloride
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-72167660c5b94f48aa76aacf57b3c998
출처 데이터셋
uspto-grants-2010_02
특허 번호
US07662402B2

반응 노트

불러오는 중…