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Potassium Carbonate → 1-(difluoromethyl)-4-ethynyl-1H-pyrazole

HRID 2205945
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HRID 2205945 반응식
[F:1][CH:2]([F:14])[N:3]1[CH:7]=[C:6]([C:8]#[C:9][Si](C)(C)C)[CH:5]=[N:4]1.C(=O)([O-])[O-].[K+].[K+]>CO>[F:1][CH:2]([F:14])[N:3]1[CH:7]=[C:6]([C:8]#[CH:9])[CH:5]=[N:4]1
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참가 물질

4

반응물 2

HCID 11430Potassium CarbonateHCID 682906451-(Difluoromethyl)-4-((trimethylsilyl)ethynyl)-1H-pyrazole

생성물 1

HCID 867063321-(difluoromethyl)-4-ethynyl-1H-pyrazole수율 72%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

1-(Difluoromethyl)-4-((trimethylsilyl)ethynyl)-1H-pyrazole (Preparation 151, 413 mg, 1.9 mmole) was stirred with methanol (4 mL). Potassium carbonate (17 mg) was added and stirred at room temperature for 50 minutes. The solvent was evaporated and the residue was filtered in dichloromethane through a short pad of silica to afford the title compound (187 mg 1.31 mmole 72%). 1H-NMR (CDCl3, 500 MHz): δ 3.08 (s, 1H), 7.17 (t, J=60.5 Hz, 1H), 7.75 (s, 1H), 7.97 (s, 1H).

후처리

  1. customThe solvent was evaporated
  2. filtrationthe residue was filtered in dichloromethane through a short pad of silica

출처 및 근거

ORD 기록
ord-a7eac286688e4b9d9596b38ba463631b
출처 데이터셋
uspto-grants-2016_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09371319B2

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