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

HRID 2357901노트

반응식

HRID 2357901 반응식
[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

참가 물질

4

반응물 1

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

생성물 1

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

시약·촉매·용매 2

HCID 178418406HCID 178418406, 화합물촉매HCID 6344Dichloromethane용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-c6d8234b0c7f48da8c6cc899aff1e09b
출처 데이터셋
uspto-grants-2010_07
특허 번호
US07763617B2

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