Carbon Disulfide → 5-Fluorobenzoxazole-2-thiol

HRID 70126노트

반응식

HRID 70126 반응식
[NH2:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[OH:9].[OH-].[K+].[C:12](=S)=[S:13]>CCO>[F:8][C:6]1[CH:5]=[CH:4][C:3]2[O:9][C:12](=[S:13])[NH:1][C:2]=2[CH:7]=1

참가 물질

5

반응물 3

HCID 6348Carbon DisulfideHCID 14797Potassium HydroxideHCID 27359172-Amino-4-fluorophenol

생성물 1

HCID 107972085-Fluorobenzoxazole-2-thiol

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

2-Amino-4-fluorophenol (1.21 g, 9.52 mmol) and potassium hydroxide (0.64 g, 11.4 mmol) were dissolved in carbon disulfide (15 mL) and EtOH (25 mL), and the reaction mixture was heated to reflux overnight. Upon cooling to rt, the reaction mixture was concentrated under reduced pressure. The resulting solid was suspended in 1 M aqueous HCl and collected by filtration. This was washed with 1 M aqueous HCl (2×) and water (2×) and was air-dried. This gave 1.115 g (69%) of the title compound as a yellow solid. LC-MS: RT=6.89 min., [M+H]+=169.9.

후처리

  1. temperatureto reflux overnight
  2. concentrationthe reaction mixture was concentrated under reduced pressure
  3. filtrationcollected by filtration
  4. washThis was washed with 1 M aqueous HCl (2×) and water (2×)
  5. customwas air-dried

출처 및 근거

ORD 기록
ord-c673d7e01faa4150a637bcd8bf947dcf
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08822472B2

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