Water → 5-iodo-4-methyl-7-triisopropylsilanyl-7H-pyrrolo[2,3-d]pyrimidine

HRID 509931노트

반응식

HRID 509931 반응식
[I:1][C:2]1[C:10]2[C:9]([CH3:11])=[N:8][CH:7]=[N:6][C:5]=2[NH:4][CH:3]=1.[H-].[Na+].[CH:14]([Si:17](Cl)([CH:21]([CH3:23])[CH3:22])[CH:18]([CH3:20])[CH3:19])([CH3:16])[CH3:15].O>O1CCCC1>[I:1][C:2]1[C:10]2[C:9]([CH3:11])=[N:8][CH:7]=[N:6][C:5]=2[N:4]([Si:17]([CH:21]([CH3:23])[CH3:22])([CH:18]([CH3:20])[CH3:19])[CH:14]([CH3:16])[CH3:15])[CH:3]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 24758Sodium hydrideHCID 139400Triisopropylsilyl chlorideHCID 582592995-iodo-4-methyl-7H-pyrrolo[2,3-d]pyrimidine

생성물 1

HCID 582589665-iodo-4-methyl-7-triisopropylsilanyl-7H-pyrrolo[2,3-d]pyrimidine

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To 5-iodo-4-methyl-7H-pyrrolo[2,3-d]pyrimidine (19, 323.6 mg, 1.25 mmol) in 8 mL of tetrahydrofuran under nitrogen, sodium hydride (57.41 mg, 60% in mineral oil, 1.44 mmol) was added. The reaction was stirred at room temperature for 10 minutes, then triisopropysilyl chloride (3, 0.304 mL, 1.44 mmol) was added. The reaction was stirred at room temperature for 2 hours, then poured into water and extracted with ethyl acetate. The organic layer was dried over sodium sulfate, filtered and the filtrate concentrated under vacuum to provide the desired compound.

후처리

  1. stirringThe reaction was stirred at room temperature for 2 hours
  2. extractionextracted with ethyl acetate
  3. dry with materialThe organic layer was dried over sodium sulfate
  4. filtrationfiltered
  5. concentrationthe filtrate concentrated under vacuum

출처 및 근거

ORD 기록
ord-898767a6d296432ba01713f3e587d277
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09096593B2

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