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Methyl iodide → HCID 178503574、化合物

HRID 324478
ノート
印刷プレビュー

反応式

HRID 324478 の反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[CH:15]([C:16]3[C:17](=[S:23])[NH:18][C:19](=[O:22])[NH:20][CH:21]=3)[C:10]3[N:11]=[C:12]([CH3:14])[S:13][C:9]=3[CH:8]=[CH:7][C:6]=2[CH:24]=1.[C:25](=O)(O)[O-].[Na+].CI>C(O)C.O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[CH:15]([C:16]3[C:17]([S:23][CH3:25])=[N:18][C:19](=[O:22])[NH:20][CH:21]=3)[C:10]3[N:11]=[C:12]([CH3:14])[S:13][C:9]=3[CH:8]=[CH:7][C:6]=2[CH:24]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 6328Methyl iodide2 回HCID 516892Sodium BicarbonateHCID 88152155HCID 88152155、化合物

生成物 1

HCID 178503574HCID 178503574、化合物

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

反応条件

温度
50 °C

実験手順

A suspension of the product from example 38, step (v) (1.8 g) in ethanol (200 ml) and sodium bicarbonate (0.5 g) in water (15 ml) was heated until a complete solution formed. After cooling to room temperature methyl iodide (0.33 ml) was added and the whole stirred for 18 h. Another aliquot of methyl iodide was added (0.2 ml) followed by heating at 50° C. for 4 h. The reaction mixture was concentrated under reduced pressure and then partitioned between dichloromethane and brine. The organic phase was collected, dried (MgSO4) and evaporated under reduced pressure to leave a beige foam. Purification was by chromatography eluting with ethyl acetate/methanol mixtures to give the subtitle product as colourless solid.

後処理

  1. temperaturewas heated until a complete solution
  2. customformed
  3. additionwas added
  4. concentrationThe reaction mixture was concentrated under reduced pressure
  5. custompartitioned between dichloromethane and brine
  6. customThe organic phase was collected
  7. dry with materialdried (MgSO4)
  8. customevaporated under reduced pressure
  9. customto leave a beige foam
  10. customPurification
  11. washeluting with ethyl acetate/methanol

出典と根拠

ORDレコード
ord-ce7066069a78420da825cc22f47f2410
出典データセット
uspto-grants-2001_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06218376B1

反応ノート

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