Hydrochloric Acid → (4-(Trifluoromethoxy)benzyl)malononitrile

HRID 749601노트

반응식

HRID 749601 반응식
[F:1][C:2]([F:17])([F:16])[O:3][C:4]1[CH:15]=[CH:14][C:7]([CH:8]=[C:9]([C:12]#[N:13])[C:10]#[N:11])=[CH:6][CH:5]=1.[BH4-].[Na+].Cl>O1CCCC1.C(O)C>[F:1][C:2]([F:16])([F:17])[O:3][C:4]1[CH:5]=[CH:6][C:7]([CH2:8][CH:9]([C:12]#[N:13])[C:10]#[N:11])=[CH:14][CH:15]=1

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 8456624-(Trifluoromethoxy)benzalmalononitrileHCID 4311764Sodium borohydride

생성물 1

HCID 22235052(4-(Trifluoromethoxy)benzyl)malononitrile수율 83.6%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 8028Tetrahydrofuran용매

실험 절차

Then, 2.61 g of (4-(trifluoromethoxy)benzylidene)malononitrile was dissolved in 20 ml of tetrahydrofuran, and while stirring at room temperature, a suspension of 0.11 g of sodium borohydride in 5 ml of ethanol was added dropwise, followed by stirring at room temperature for 30 minutes. Then, 10% hydrochloric acid was added, and the mixture was extracted with diethyl ether. The organic layer was successively washed with 10% hydrochloric acid, a saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to give 2.20 g of (4-(trifluoromethoxy)benzyl)malononitrile (the intermediate (7)).

후처리

  1. additionwas added dropwise
  2. stirringby stirring at room temperature for 30 minutes
  3. extractionthe mixture was extracted with diethyl ether
  4. washThe organic layer was successively washed with 10% hydrochloric acid
  5. dry with materiala saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate
  6. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-74ddbc1f80bb47f09eac7b2d43ac95e3
출처 데이터셋
uspto-grants-2008_07
특허 번호
US07402691B2

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