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2-Chloroacrylonitrile → HCID 13361511, 화합물

HRID 1788747
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HRID 1788747 반응식
[C:1]([NH:4][C@@H:5]1[CH2:10][CH2:9][CH2:8][CH2:7][C@H:6]1[Hg]Cl)(=[O:3])[CH3:2].[Cl:13][C:14](=[CH2:17])[C:15]#[N:16].[BH4-].[Na+]>C(O)C>[C:1]([NH:4][C@@H:5]1[CH2:10][CH2:9][CH2:8][CH2:7][C@H:6]1[CH2:17][CH:14]([Cl:13])[C:15]#[N:16])(=[O:3])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 701982-ChloroacrylonitrileHCID 4311764Sodium borohydrideHCID 12257140HCID 12257140, 화합물

생성물 1

HCID 13361511HCID 13361511, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

31 g of trans-1-acetamido-2-chloromercuriocyclohexane are suspended in 250 ml of 95% strength ethanol: 187 ml (4 equivalents) of 2-chloroacrylonitrile are added. While cooling in ice, a solution of 3 g of sodium borohydride in 50 ml of ethanol is added as rapidly as possible. After warming up to room temperature, the precipitated elemental mercury is filtered off with suction over kieselguhr, thoroughly washed with ethanol and the filtrate is evaporated. The residue is taken up in methylene chloride, washed three times with 1N sodium hydroxide solution to destroy the boric esters, dried over sodium sulfate and evaporated. 13 g of the title compound are obtained as a yellow oil.

후처리

  1. temperatureWhile cooling in ice
  2. filtrationthe precipitated elemental mercury is filtered off with suction over kieselguhr
  3. washthoroughly washed with ethanol
  4. customthe filtrate is evaporated
  5. washwashed three times with 1N sodium hydroxide solution
  6. customto destroy the boric esters
  7. dry with materialdried over sodium sulfate
  8. customevaporated

출처 및 근거

ORD 기록
ord-9c1a67b4b67e42289524d20455c072ac
출처 데이터셋
uspto-grants-1987_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04684662

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