Methyl iodide → 4-Bromo-2-(methoxymethyl)thiophene

HRID 501303

反応式

HRID 501303 の反応式
[H-].[Na+].[CH3:3]I.[Br:5][C:6]1[CH:7]=[C:8]([CH2:11][OH:12])[S:9][CH:10]=1>O1CCCC1>[Br:5][C:6]1[CH:7]=[C:8]([CH2:11][O:12][CH3:3])[S:9][CH:10]=1

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 2795484(4-Bromo-2-thienyl)methanol

生成物 1

HCID 150183124-Bromo-2-(methoxymethyl)thiophene

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Add sodium hydride (737 mg, 29.23 mmol, 1.10 equivalents, 95%) to a solution containing methyl iodide (1.65 mL, 26.57 mmol, 1.00 equivalents) and (4-bromo-thiophen-2-yl)-methanol (5.13 g, 26.57 mmol, 1.00 equivalents) in tetrahydrofuran (dry, 25 mL). Stir the resulting mixture at room temperature overnight and evaporate. Partition the residue between water (100 mL) and dichloromethane (100 mL). Extract the aqueous layer with dichloromethane (100 mL), combine the organic layers, dry over magnesium sulfate, filter and evaporate to yield the desired product as a yellow oil.

後処理

  1. customevaporate
  2. customPartition the residue between water (100 mL) and dichloromethane (100 mL)
  3. extractionExtract the aqueous layer with dichloromethane (100 mL)
  4. dry with materialdry over magnesium sulfate
  5. filtrationfilter
  6. customevaporate

出典と根拠

ORDレコード
ord-18807178b5ad41e58744cd1064982c73
出典データセット
uspto-grants-2010_08
特許番号
US07772252B2

関連ノート

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