4-Hydroxymethyl-7-iodo-2-trifluoromethylpyrazolo[1,5-a]pyridin → 2-Trifluoromethyl-4-formyl-7-iodo-pyrazolo[1,5-a]pyridine

HRID 2357901ノート

反応式

HRID 2357901 の反応式
[F:1][C:2]([F:16])([F:15])[C:3]1[CH:14]=[C:6]2[C:7]([CH2:12][OH:13])=[CH:8][CH:9]=[C:10]([I:11])[N:5]2[N:4]=1>ClCCl.[O-2].[O-2].[Mn+4]>[F:16][C:2]([F:1])([F:15])[C:3]1[CH:14]=[C:6]2[C:7]([CH:12]=[O:13])=[CH:8][CH:9]=[C:10]([I:11])[N:5]2[N:4]=1

参加物

4

反応物 1

HCID 593893564-Hydroxymethyl-7-iodo-2-trifluoromethylpyrazolo[1,5-a]pyridin

生成物 1

HCID 593892992-Trifluoromethyl-4-formyl-7-iodo-pyrazolo[1,5-a]pyridine収率 91.6%

試薬・触媒・溶媒 2

HCID 178418406HCID 178418406、化合物触媒HCID 6344Dichloromethane溶媒

実験手順

The compound of Example 112 (3.26 g) was dissolved in dichloromethane (50.0 mL). To this solution, activated manganese dioxide (8.29 g) was added and the mixture was stirred at room temperature for 14 hours. Subsequently, the reaction mixture was filtered through Celite and the filtrate was evaporated. Purification of the resulting residue by silica gel column chromatography (hexane:ethyl acetate=4:1) afforded the title compound as a yellow powder (2.97 g).

後処理

  1. additionwas added
  2. filtrationSubsequently, the reaction mixture was filtered through Celite
  3. customthe filtrate was evaporated
  4. customPurification of the resulting residue by silica gel column chromatography (hexane:ethyl acetate=4:1)

出典と根拠

ORDレコード
ord-c6d8234b0c7f48da8c6cc899aff1e09b
出典データセット
uspto-grants-2010_07
特許番号
US07763617B2

反応ノート

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