Sodium Bicarbonate → 3-(Methoxymethyl)-4-methylaniline

HRID 261288

反応式

HRID 261288 の反応式
[CH3:1][C:2]1[CH:10]=[CH:9][C:8]([N+:11]([O-])=O)=[CH:7][C:3]=1[CH2:4][O:5][CH3:6].O.[S-2].[Na+].[Na+].C(=O)(O)[O-].[Na+]>C(O)C.O>[CH3:6][O:5][CH2:4][C:3]1[CH:7]=[C:8]([CH:9]=[CH:10][C:2]=1[CH3:1])[NH2:11]

参加物

6

反応物 3

HCID 516892Sodium BicarbonateHCID 12767666Methyl 2-methyl-5-nitrobenzyl etherHCID 19906495Sodium sulfide monohydrate

生成物 1

HCID 127676673-(Methoxymethyl)-4-methylaniline収率 96.9%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

Methyl 2-methyl-5-nitrobenzyl ether (11.5 g) was dissolved in 125 ml of absolute ethanol. To this was added a solution of sodium sulfide monohydrate (48.3 g) and sodium bicarbonate (16.7 g) in 75 ml of water. The resulting mixture was refluxed until tlc indicated all the starting material was gone. The mixture was then concentrated in vacuo to an oily solid. Methylene chloride was added and the mixture filtered. The methylene chloride layer was separated and dried. After removal of the drying agent, the solvent was concentrated in vacuo to give 9.3 g of a mobile orange liquid.

後処理

  1. temperatureThe resulting mixture was refluxed
  2. concentrationThe mixture was then concentrated in vacuo to an oily solid
  3. additionMethylene chloride was added
  4. filtrationthe mixture filtered
  5. customThe methylene chloride layer was separated
  6. customdried
  7. customAfter removal of the drying agent
  8. concentrationthe solvent was concentrated in vacuo

出典と根拠

ORDレコード
ord-edcb9176ca00473e94e69a8f9a2a1510
出典データセット
uspto-grants-1979_08
特許番号
US04165231

関連ノート

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