Iodine → HCID 178474493、化合物

HRID 588584ノート

反応式

HRID 588584 の反応式
[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]

参加物

5

反応物 3

HCID 807IodineHCID 24345Iodic acidHCID 178474234HCID 178474234、化合物

生成物 1

HCID 178474493HCID 178474493、化合物収率 296.8%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
65 °C

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-383135e79a1244a8aff3053bb178f680
出典データセット
uspto-grants-2016_01
特許番号
US09227976B2

反応ノート

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