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Iodoethane → HCID 58268029、化合物

HRID 1615974
ノート
印刷プレビュー

反応式

HRID 1615974 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

HCID 58268029HCID 58268029、化合物収率 32.5%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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).

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  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

出典と根拠

ORDレコード
ord-c0560a184c814887ba2713b182b13373
出典データセット
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08765743B2

反応ノート

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