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Triethylamine → HCID 57736565, 화합물

HRID 536336
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HRID 536336 반응식
[Br:1][C:2]1[CH:9]=[C:8]([CH3:10])[C:7]([N+:11]([O-])=O)=[CH:6][C:3]=1[C:4]#[N:5].[Sn](Cl)(Cl)(Cl)Cl.C(N(CC)CC)C>C(O)C>[NH2:11][C:7]1[C:8]([CH3:10])=[CH:9][C:2]([Br:1])=[C:3]([CH:6]=1)[C:4]#[N:5]
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참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 24287Tin tetrachlorideHCID 57736551HCID 57736551, 화합물

생성물 1

HCID 57736565HCID 57736565, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a solution of 2-bromo-4-methyl-5-nitrobenzonitrile (500 mg, 2.07 mmol) in ethanol (20 mL) was added tin chloride (785 mg, 4.14 mmol). The mixture was refluxed for 5 h. After cooling to room temperature, triethylamine (1.01 g, 10 mmol) was added. The mixture was concentrated and purified by silica chromatography (30-50% ethyl acetate in hexanes gradient) to afford 5-Amino-2-bromo-4-methylbenzonitrile a as beige solid; ESMS m/z 211 (M+H+).

후처리

  1. temperatureThe mixture was refluxed for 5 h
  2. concentrationThe mixture was concentrated
  3. custompurified by silica chromatography (30-50% ethyl acetate in hexanes gradient)

출처 및 근거

ORD 기록
ord-08a4db77db524e80bf66e24c45ad1438
출처 데이터셋
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08859574B2

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