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Potassium Carbonate → HCID 83826394, 화합물

HRID 926379
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HRID 926379 반응식
[CH3:1][O:2][C:3]1[N:4]=[CH:5][C:6]([C:9]#[N:10])=[N:7][CH:8]=1.[CH3:11][Mg]Br.[BH4-].[Na+].[Cl-].[NH4+].C(=O)([O-])[O-].[K+].[K+]>O1CCCC1>[CH3:1][O:2][C:3]1[N:4]=[CH:5][C:6]([CH:9]([NH2:10])[CH3:11])=[N:7][CH:8]=1
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참가 물질

7

반응물 5

HCID 11430Potassium CarbonateHCID 25517Ammonium ChlorideHCID 4311764Sodium borohydrideHCID 534389935-Methoxypyrazine-2-carbonitrileHCID 178418573HCID 178418573, 화합물

생성물 1

HCID 83826394HCID 83826394, 화합물수율 4.4%

시약·촉매·용매 1

HCID 8028
Tetrahydrofuran
용매

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온도
25 °C

실험 절차

To a solution of 5-methoxy-pyrazine-2-carbonitrile (1.0 g, 7.4 mmol) in tetrahydrofuran at −78° C. was added dropwise 1 M methylmagnesium bromide (8.14 ml, 8.14 mmol) and the mixture was stirred for 1 h at 25° C. Sodium borohydride (250 mg, 6.62 mmol) was added at −78° C. and the mixture was allowed to warm to 25° C. Aqueous ammonium chloride was added and after addition of excess potassium carbonate the mixture was extracted 3 times with dichloromethane, solvents were evaporated to give 0.05 g (4%) of crude 1-(5-methoxy-pyrazin-2-yl)-ethylamine. LC/MS (method 5): Rt=1.26 min; m/z=154.15 (M+H+).

후처리

  1. temperatureto warm to 25° C
  2. extractionwas extracted 3 times with dichloromethane, solvents
  3. customwere evaporated

출처 및 근거

ORD 기록
ord-51cec6153e5848f694da46ba6046785f
출처 데이터셋
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09284333B2

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