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2-Chloro-4-fluorophenylacetonitrile → Ammonia

HRID 494430
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HRID 494430 반응식
[BH4-].[Na+].[Cl:3][C:4]1[CH:9]=[C:8]([F:10])[CH:7]=[CH:6][C:5]=1[CH2:11][C:12]#[N:13]>CO.O.O.O.O.O.O.[Co](Cl)Cl>[NH3:13].[Cl:3][C:4]1[CH:9]=[C:8]([F:10])[CH:7]=[CH:6][C:5]=1[CH2:11][CH2:12][NH2:13]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 2

HCID 27250632-Chloro-4-fluorophenylacetonitrileHCID 4311764Sodium borohydride

생성물 2

HCID 222AmmoniaHCID 218881112-(2-Chloro-4-fluorophenyl)ethan-1-amine

시약·촉매·용매 2

HCID 517166Dichlorocobalt hexahydrate촉매HCID 887Methanol용매

실험 절차

Sodium borohydride (1.73 g, 45.51 mmol) was added portionwise to a solution of 2-chloro-4-fluorophenylacetonitrile (1.04 g, 6.15 mmol) and cobalt (II) chloride hexahydrate (2.18 g, 9.22 mmol) in methanol (30 mL) and the mixture was stirred at room temperature for 3 hours. The suspension was then filtered though Celite®, concentrated in vacuo and the residue was partitioned between 1M hydrochloric acid (40 mL) and dichloromethane (40 mL). The aqueous phase was separated, basified to pH 11 with 1M ammonia solution and extracted with dichloromethane (2×40 mL). The combined organic solution was washed with brine (30 mL), dried over magnesium sulfate and concentrated in vacuo. The residue was purified by column chromatography on silica gel, eluting with dichloromethane:methanol:0.88 ammonia, 100:0:0 to 98:2:0.2, to afford the title compound as a yellow oil, 350 mg.

후처리

  1. filtrationThe suspension was then filtered though Celite®
  2. concentrationconcentrated in vacuo
  3. customthe residue was partitioned between 1M hydrochloric acid (40 mL) and dichloromethane (40 mL)
  4. customThe aqueous phase was separated
  5. extractionextracted with dichloromethane (2×40 mL)
  6. washThe combined organic solution was washed with brine (30 mL)
  7. dry with materialdried over magnesium sulfate
  8. concentrationconcentrated in vacuo
  9. customThe residue was purified by column chromatography on silica gel
  10. washeluting with dichloromethane

출처 및 근거

ORD 기록
ord-11d727eb596642eeb93a3363e9fdedd9
출처 데이터셋
uspto-grants-2009_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07538141B2

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