Sodium Methoxide → HCID 23144869、化合物

HRID 1875560ノート

反応式

HRID 1875560 の反応式
C[O-].[Na+].Br[CH2:5][C:6]1[C:7]([N+:16]([O-:18])=[O:17])=[C:8]([CH:13]=[CH:14][CH:15]=1)[C:9]([O:11][CH3:12])=[O:10].[O:19]1CCOC[CH2:20]1.Cl>CO>[CH3:20][O:19][CH2:5][C:6]1[C:7]([N+:16]([O-:18])=[O:17])=[C:8]([CH:13]=[CH:14][CH:15]=1)[C:9]([O:11][CH3:12])=[O:10]

参加物

5

反応物 3

HCID 10942334Sodium MethoxideHCID 204431481,4-Dioxane hydrochlorideHCID 22509333Methyl 3-(bromomethyl)-2-nitrobenzoate

生成物 1

HCID 23144869HCID 23144869、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

Methanol solution (4.7 mL) of sodium methoxide (197 mg) was added dropwise into the mixture of methyl 3-bromomethyl-2-nitrobenzoate (1 g) and methanol (7 mL) under heating and refluxing. Two minutes later, the mixture was cooled down with ice and 1.82 mL of 4M hydrogen chloride dioxane solution was added dropwise thereto. After removing the solvent, diethylether and water were added and the organic layer thereof was dried over sodium sulfate. After removing the solvent, the obtained residue was purified with silica gel column chromatography to obtain 621 mg of methyl 3-methoxymethyl-2-nitrobenzoate.

後処理

  1. temperatureunder heating
  2. temperaturerefluxing
  3. additionwas added dropwise
  4. customAfter removing the solvent, diethylether and water
  5. additionwere added
  6. dry with materialthe organic layer thereof was dried over sodium sulfate
  7. customAfter removing the solvent
  8. customthe obtained residue was purified with silica gel column chromatography

出典と根拠

ORDレコード
ord-4740903a398f405eb2e1492264a24046
出典データセット
uspto-grants-2012_11
特許番号
US08309561B2

反応ノート

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