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2-Amino-4-chlorophenol → HCID 86086750, 화합물

HRID 1189071
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HRID 1189071 반응식
[CH3:1][O:2][C:3](=[NH:8])[CH2:4][CH2:5][C:6]#[CH:7].N[C:10]1[CH:15]=[C:14]([Cl:16])[CH:13]=[CH:12]C=1O>ClC(Cl)C>[CH2:4]([C:3]1[O:2][C:1]2[CH:10]=[CH:15][C:14]([Cl:16])=[CH:13][C:12]=2[N:8]=1)[CH2:5][C:6]#[CH:7]
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참가 물질

4

반응물 2

HCID 72652-Amino-4-chlorophenolHCID 57691793Methyl pent-4-ynimidate

생성물 1

HCID 86086750HCID 86086750, 화합물수율 7%

시약·촉매·용매 1

HCID 63651,1-Dichloroethane용매

실험 절차

A mixture of pent-4-ynimidic acid methyl ester (142 mg, 1.28 mmol) and 2-amino-4-chlorophenol (227 mg, 1.53 mmol) in dichloroethane (10 mL) was stirred for 2 days under reflux. The solvent was evaporated, the residue was partly dissolved in MeOH and filtered. The filtrate was concentrated, and the resulting crude residue was purified by flash chromatography (cyclohexane/AcOEt 9:1) to yield 18 mg (87 μmol, 7%) of 2-(but-3-ynyl)-5-chlorobenzo[d]oxazole.

후처리

  1. temperatureunder reflux
  2. customThe solvent was evaporated
  3. dissolutionthe residue was partly dissolved in MeOH
  4. filtrationfiltered
  5. concentrationThe filtrate was concentrated
  6. customthe resulting crude residue was purified by flash chromatography (cyclohexane/AcOEt 9:1)

출처 및 근거

ORD 기록
ord-275d77ccbccc49b99777bc75c38a400b
출처 데이터셋
uspto-grants-2014_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08674106B2

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