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Iodoethane → HCID 58268029, 화합물

HRID 1615974
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HRID 1615974 반응식
[Br:1][C:2]1[CH:3]=[C:4]([NH2:11])[C:5]2[CH:6]=[N:7][NH:8][C:9]=2[CH:10]=1.[H-].[Na+].I[CH2:15][CH3:16]>C1COCC1>[Br:1][C:2]1[CH:3]=[C:4]([NH2:11])[C:5]2[CH:6]=[N:7][N:8]([CH2:15][CH3:16])[C:9]=2[CH:10]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6340IodoethaneHCID 24758Sodium hydrideHCID 247280636-Bromo-1H-indazol-4-amine

생성물 1

HCID 58268029HCID 58268029, 화합물수율 32.5%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 6-bromo-1H-indazol-4-amine (available from Sinova, 300 mg, 1.41 mmol) in THF (7 ml), cooled to 0° C. was added 60% sodium hydride in mineral oil (62 mg, 1.55 mmol) and the reaction was stirred for 15 mins. Iodoethane (0.124 ml, 1.55 mmol) was added and the reaction was stirred overnight. The reaction was quenched with MeOH (1 ml), diluted with water (10 ml), then extracted into ethyl acetate, which was separated and evaporated to dryness. The residue was purified by silica chromatography using 0-100% ethyl acetate in cyclohexane over 80 mins. Pure fractions were evaporated to give the title compound (110 mg).

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후처리

  1. stirringthe reaction was stirred overnight
  2. customThe reaction was quenched with MeOH (1 ml)
  3. additiondiluted with water (10 ml)
  4. extractionextracted into ethyl acetate, which
  5. customwas separated
  6. customevaporated to dryness
  7. customThe residue was purified by silica chromatography
  8. customover 80 mins
  9. customPure fractions were evaporated

출처 및 근거

ORD 기록
ord-c0560a184c814887ba2713b182b13373
출처 데이터셋
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08765743B2

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