Hydrochloric Acid → HCID 11687105, 화합물

HRID 1743620노트

반응식

HRID 1743620 반응식
[Cl:1][C:2]1[CH:14]=[CH:13][C:5]([C:6](=[C:8]([C:11]#[N:12])[C:9]#[N:10])[CH3:7])=[CH:4][CH:3]=1.[BH4-].[Na+].Cl>C(O)C>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([CH:6]([CH:8]([C:9]#[N:10])[C:11]#[N:12])[CH3:7])=[CH:13][CH:14]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 2636762-[1-(4-chlorophenyl)ethylidene]malononitrileHCID 4311764Sodium borohydride

생성물 1

HCID 11687105HCID 11687105, 화합물수율 56.1%

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

First, 3.00 g of (4-chloro-α-methylbenzylidene)malononitrile was dissolved in 20 ml of ethanol, and while stirring at room temperature, a suspension of 0.15 g of sodium borohydride in 5 ml of ethanol was added dropwise, followed by stirring at room temperature for 30 minutes. Then, 10% hydrochloride acid was added to the reaction mixture, which 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 1.70 g of (1-(4-chlorophenyl)ethyl)malononitrile (the intermediate (6)).

후처리

  1. additionwas added dropwise
  2. stirringby stirring at room temperature for 30 minutes
  3. extractionwas 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-9594f4c33b6042109ef0f7c8586cba83
출처 데이터셋
uspto-grants-2006_03
특허 번호
US07011838B2

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