Iodine → HCID 178474493, 화합물

HRID 2205786노트

반응식

HRID 2205786 반응식
[F:1][C:2]([F:13])([F:12])[C:3]1[CH:7]=[C:6]([NH:8][C:9](=[O:11])[CH3:10])[NH:5][N:4]=1.[I:14](O)(=O)=O.II>C(O)C>[I:14][C:7]1[C:3]([C:2]([F:1])([F:12])[F:13])=[N:4][NH:5][C:6]=1[NH:8][C:9](=[O:11])[CH3:10]

참가 물질

5

반응물 3

HCID 807IodineHCID 24345Iodic acidHCID 178474234HCID 178474234, 화합물

생성물 1

HCID 178474493HCID 178474493, 화합물수율 296.8%

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
65 °C

실험 절차

To a solution of N-[3-(trifluoromethyl)-1H-pyrazol-5-yl]acetamide (7.3 g, 38 mmol) in ethanol (120 mL) were added iodic acid (1.65 g, 9.4 mmol) and iodine (4.8 g, 18.9 mmol). The reaction was stirred for 3.25 h at 65° C. The reaction mixture was concentrated in vacuo and the residue was suspended in hot CH2Cl2 (150 ml) with stirring, the solid was filtered and resuspended in hot CH2Cl2 (100 ml) filtered and dried in vacuo to provide the title compound as a white solid (8.9 g) which was used in the subsequent step.

후처리

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. stirringwith stirring
  3. filtrationthe solid was filtered
  4. filtrationfiltered
  5. customdried in vacuo

출처 및 근거

ORD 기록
ord-0c356b24862c48968f3189135ba00be4
출처 데이터셋
uspto-grants-2016_06
특허 번호
US09371332B2

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